CN111234429A - PTFE/boron nitride composite material and preparation method thereof - Google Patents
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- 229920001343 polytetrafluoroethylene Polymers 0.000 title claims abstract description 73
- 239000004810 polytetrafluoroethylene Substances 0.000 title claims abstract description 73
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 title claims abstract description 49
- 229910052582 BN Inorganic materials 0.000 title claims abstract description 41
- 239000002131 composite material Substances 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 238000005245 sintering Methods 0.000 claims abstract description 28
- 238000000034 method Methods 0.000 claims abstract description 19
- 238000002156 mixing Methods 0.000 claims abstract description 19
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000002135 nanosheet Substances 0.000 claims abstract description 13
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 11
- 239000011812 mixed powder Substances 0.000 claims abstract description 11
- 239000000843 powder Substances 0.000 claims abstract description 11
- 238000003825 pressing Methods 0.000 claims abstract description 11
- 229920002545 silicone oil Polymers 0.000 claims abstract description 10
- 239000007791 liquid phase Substances 0.000 claims abstract description 9
- -1 polytetrafluoroethylene Polymers 0.000 claims abstract description 8
- 238000005406 washing Methods 0.000 claims abstract description 8
- 238000001914 filtration Methods 0.000 claims abstract description 7
- 239000000839 emulsion Substances 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000010438 heat treatment Methods 0.000 claims description 17
- 230000008569 process Effects 0.000 claims description 11
- 238000001816 cooling Methods 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 claims description 2
- 238000007723 die pressing method Methods 0.000 claims 1
- 238000000465 moulding Methods 0.000 abstract description 5
- 238000003756 stirring Methods 0.000 abstract description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- 239000006185 dispersion Substances 0.000 description 6
- 229910021389 graphene Inorganic materials 0.000 description 6
- 239000000945 filler Substances 0.000 description 4
- 238000011049 filling Methods 0.000 description 4
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- 239000000463 material Substances 0.000 description 4
- 230000009471 action Effects 0.000 description 3
- 239000007822 coupling agent Substances 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 125000001153 fluoro group Chemical group F* 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000000967 suction filtration Methods 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 239000002113 nanodiamond Substances 0.000 description 2
- 229920000620 organic polymer Polymers 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229910002971 CaTiO3 Inorganic materials 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229920002313 fluoropolymer Polymers 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 239000011256 inorganic filler Substances 0.000 description 1
- 229910003475 inorganic filler Inorganic materials 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 238000010907 mechanical stirring Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 238000002715 modification method Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 230000007480 spreading Effects 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/38—Boron-containing compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/38—Boron-containing compounds
- C08K2003/382—Boron-containing compounds and nitrogen
- C08K2003/385—Binary compounds of nitrogen with boron
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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Abstract
The invention discloses a PTFE/boron nitride composite material and a preparation method thereof. The composite material is prepared by firstly obtaining mixed powder by adopting a liquid phase mixing method and then carrying out cold pressing and sintering. The method sequentially comprises the following steps: 1) stripping of Boron Nitride (BN): treating hexagonal boron nitride powder with molten citric acid for 24h, washing with water to neutrality, filtering, and drying to obtain boron nitride nanosheet (n-BN); 2) polytetrafluoroethylene (PTFE) and n-BN: respectively dispersing PTFE powder and boron nitride nanosheets (n-BN) in silicone oil to form stable emulsion, intensively and uniformly stirring and mixing, filtering, washing with dichloromethane, and drying to obtain mixed powder; 3) cold press molding and sintering: and putting the mixed powder into a mould pressing die, carrying out cold pressing under a certain pressure, taking out the parison, putting the parison into a sintering furnace, and sintering according to a certain temperature curve to finally obtain the PTFE/boron nitride composite material. The liquid phase mixing method adopted by the invention effectively improves the mixing uniformity, and the prepared PTFE/boron nitride composite material has excellent wear resistance and heat conductivity.
Description
Technical Field
The invention relates to a PTFE/boron nitride composite material and a preparation method thereof, and particularly provides a method for preparing the PTFE/boron nitride composite material by liquid phase mixing and cold pressure sintering.
Background
Polytetrafluoroethylene (PTFE) has excellent chemical stability, radiation resistance, dielectric properties, and extremely low coefficient of friction and self-lubricity, and is one of the most advanced and widely used resins in fluoroplastics. It has wide application in the fields of machinery, chemistry, chemical engineering, electronics, electricity and the like, and has great application value in the fields of space navigation and military. However, due to the structural characteristics of PTFE molecules, attraction among macromolecules is small, and the ribbon crystal is easy to peel off in a sheet shape, so that the defects of poor mechanical property, poor creep resistance, easiness in cold flow, poor rebound resilience, no wear resistance, no conductivity, no heat conduction, large linear expansion coefficient and the like are shown, and the wide application of the PTFE in certain industries is greatly limited. Therefore, the intensive research on the structure and physical and chemical properties of polytetrafluoroethylene, especially the development of novel PTFE materials with excellent comprehensive properties through chemical and physical modification, has become the main direction of research and development of polytetrafluoroethylene at present. The filling modification of inorganic nano-filler is one of the most common modification methods of polytetrafluoroethylene.
The inorganic nano-filler for filling modified PTFE at present mainly comprises nano-diamond and CaCO3、CaTiO3Carbon nanotubes, graphene, and the like. Marcus et al filled PTFE with glass fiber, the friction and wear performance of the composite material was improved relatively, however Lim et al added 2% nanodiamond to PTFE obtained the minimum friction coefficient and wear damage. Modified CaCO for caixiong and the like3The polytetrafluoroethylene is filled to improve the mechanical property. However, these reports all suffer from the problem of the filler not being mixed uniformly enough with the PTFE matrix. Songyong et al improve the mixing uniformity of the filler and the matrix by adding a coupling agent, but the addition of the coupling agent causes complication of the preparation process and aggravates environmental pollution, and high temperature conditions may cause decomposition of the coupling agent during the subsequent sintering of PTFE. According to Xuezhen and the like, the PTFE is filled with graphene, the graphene is firstly carboxylated and aminated, and then is compounded with the PTFE to supply electricity to the surface of a power supply groupThe sub-clouds will be biased towards fluorine atoms, i.e. towards PTFE. Under the action of van der waals force, electron cloud flow generated by an induction effect enhances the interface adhesive force between the graphene and the PTFE, and the performance of the PTFE can be improved to a certain extent. However, such intermolecular forces are relatively small, and thus the improvement in performance is limited.
As a two-dimensional material with a structure similar to graphene, hexagonal boron nitride nanosheets (n-BN) are a very promising filling material, have very good thermal conductivity, and have thermal conductivity superior to that of most metal and ceramic materials. And as the thickness of the sheet layer is reduced, the value of the thermal conductivity is increased, and the thermal conductivity of the single-layer BN nano sheet is larger than that of the multi-layer and bulk BN. In addition, n-BN, like graphene, is a nanomaterial with very good mechanical strength. Just because of its extremely high thermal conductivity and good mechanical properties, n-BN has been widely used as a two-dimensional inorganic filler for organic polymers to improve the thermal conductivity and mechanical properties of the organic polymers.
Hexagonal boron nitride can have a good modification effect on PTFE, but currently, the adopted hexagonal boron nitride is mainly bulk BN, which easily causes uneven structure of the composite material and instead becomes a stress concentration point, and reduces the use performance of the material. In addition, the BN filling modified PTFE reported at present basically adopts high-speed mechanical mixing of two raw materials, and then cold pressing and sintering of mixed powder are carried out. The mechanical mixing is difficult to be uniform, and in the sintering process, the PTFE molecular chain can generate thermal motion, which is likely to cause the aggregation of BN, thus causing the non-uniformity of the composite material structure and influencing the performance of the composite material.
According to the problems in the prior art, in order to improve the mechanical property, frictional wear property and heat conductivity of PTFE, the project adopts BN nano-sheets to modify PTFE: (1) the B-N bond of the block BN is broken by adopting molten citric acid to carry out heat treatment on the block BN, so that a large number of B, N vacancy defects are caused, which is favorable for forming-OH and-NH-functional groups at the defects and edges of the boron nitride nanosheet layer, and the boron nitride layer is spread at intervals, so that the nanosheet is obtained. (2) The large electronegativity of fluorine atoms in PTFE and hydrogen atoms in silicone oil is poor, so that strong dipole interaction is caused, and PTFE powder can be dispersed in the silicone oil to form stable emulsion. And the boron nitride can also be dispersed in the silicone oil to form emulsion, and the liquid phase mixing is adopted, which is more favorable for uniform dispersion than the solid phase mixing. In addition, the B atoms on the surface of the peeled n-BN have empty orbitals, and the fluorine atoms of the PTFE have unpaired electrons, so that the two can generate coordination action, and the uniform mixing of the PTFE and the n-BN is also facilitated. (3) Because the viscosity of PTFE is very high when the PTFE is molten, the composite material is prepared by adopting a cold-pressing sintering molding process. The PTFE and n-BN in the composite material obtained in the way have better dispersion effect, and the composite material with excellent performance can be obtained.
Disclosure of Invention
The invention aims to provide a method for preparing a PTFE/boron nitride composite material by combining liquid phase mixing with cold-pressing sintering, which comprises the following components in percentage by mass:
PTFE：90-99 wt%；
boron nitride: 1-10 wt%.
The preparation method of the PTFE/boron nitride composite material is characterized by comprising the following steps:
(1) stripping of Boron Nitride (BN)
Treating hexagonal boron nitride powder with molten citric acid for 24h, washing with water to neutrality, filtering, and drying to obtain boron nitride nanosheet (n-BN);
(2) liquid phase mixing of PTFE and n-BN
Weighing PTFE and n-BN according to a proportion, respectively dispersing PTFE powder and boron nitride nanosheets (n-BN) in silicone oil to form stable emulsion, uniformly mixing, filtering, washing with dichloromethane, and drying to obtain mixed powder;
(3) cold press forming and sintering
Placing the mixed powder into a die, performing cold press molding under pressure, and maintaining the pressure for a period of time; and then the shaped blank is placed into a sintering furnace, sintering is carried out according to a certain temperature control program, and the product is obtained after sintering is completed and furnace cooling is carried out.
The PTFE/boron nitride composite material is characterized in that: the grain diameter of the hexagonal boron nitride is 1-10 mu m.
The PTFE/boron nitride composite material is characterized in that: the polytetrafluoroethylene is suspended fine powder with the particle size of 20-80 mu m.
The PTFE/boron nitride composite material is characterized in that: in the step 1), the reaction temperature is 160-180 ℃.
The PTFE/boron nitride composite material is characterized in that: in the step 2), the mass fraction of n-BN is 1-10 wt%.
The PTFE/boron nitride composite material is characterized in that: in the step 3), the cold pressing pressure is 100-140 MPa.
The PTFE/boron nitride composite material is characterized in that: in the step 3), during the sintering process, the temperature control program is as follows:
I. the heating rate is 1.5 ℃/min, the target temperature is 130 ℃, and the temperature is kept for 1 h;
II, heating up at a rate of 1.4 ℃/min, keeping the target temperature at 250 ℃ for 1 h;
III, heating up at a rate of 1.1 ℃/min, keeping the temperature at the target temperature of 327 ℃ for 2 h;
IV, heating up at a rate of 1 ℃/min, keeping the temperature at 345 ℃ for 1 h;
v, the heating rate is 0.4 ℃/min, the target temperature is 375 ℃, and the temperature is kept for 1-5 h;
and VI, cooling along with the furnace.
Detailed Description
The invention will be further described with reference to specific examples, but the scope of the invention is not limited thereto.
Examples 1-4, the composition and process parameters are given in Table 1.
The preparation method of the composite material comprises the following steps:
(1) stripping of Boron Nitride (BN)
Treating hexagonal boron nitride powder with molten citric acid for 24h, washing with water to neutrality, filtering, and drying to obtain hexagonal boron nitride nanosheets (n-BN);
(2) liquid phase mixing of PTFE and n-BN
Weighing a certain amount of PTFE powder, mixing the PTFE powder with silicone oil, and mechanically stirring for about 1h to uniformly disperse the PTFE in the silicone oil; a certain amount of n-BN powder is weighed, and silicone oil is used as a medium to form a good dispersion under the action of mechanical stirring. Finally, the two dispersions are mixed together to form a uniformly dispersed mixed liquid. Carrying out suction filtration on the uniformly stirred dispersion liquid, washing residual silicone oil in the powder by using dichloromethane after the dispersion liquid is subjected to suction filtration to a certain degree, putting the powder into an iron plate for further drying after the mixed powder is basically subjected to suction filtration and drying, and drying in a drying oven at 150 ℃ for 4-5 hours;
(3) cold press forming and sintering
Weighing a certain amount of completely dried mixed powder, uniformly spreading the mixed powder in a mould so as to expect that the sample is uniformly stressed and the green body has uniform density in the pressing process, and then pressing the sample on a flat vulcanizing machine at a certain pressure. And after the molding is finished, taking out the sample in the mold. Sintering is the most critical step in the whole sample preparation process, and the sintering process is the most direct influence factor on the performance of the composite material. After a plurality of experiments, the following sintering process is adopted for summary and conclusion, and is more suitable:
1) because the round hole is great on the iron disc of fritting furnace, for avoiding producing the influence in the sample sintering process, it is 0.8 mm to stack up the aperture under the sample, and thickness is 0.8 mm's iron sheet. Starting the sintering furnace, and simultaneously opening the rotary table and blowing air to ensure that the sample is uniformly heated in the sintering furnace;
2) because PTFE has poor thermal conductivity, if the temperature rise rate during sintering is not strictly controlled, the sample will be greatly affected. Thus, throughout the experimental sintering process, the temperature control procedure was as follows:
I. the heating rate is 1.5 ℃/min, the target temperature is 130 ℃, and the temperature is kept for 1 h;
II, heating up at a rate of 1.4 ℃/min, keeping the target temperature at 250 ℃ for 1 h;
III, heating up at a rate of 1.1 ℃/min, keeping the temperature at the target temperature of 327 ℃ for 2 h;
IV, heating up at a rate of 1 ℃/min, keeping the temperature at 345 ℃ for 1 h;
v, the heating rate is 0.4 ℃/min, the target temperature is 375 ℃, and the temperature is kept for 1-5 h;
and VI, cooling along with the furnace.
(4) The finished product was subjected to performance tests, the test results are shown in table 2. The prepared PTFE/boron nitride composite material has excellent wear resistance and heat conductivity.
TABLE 1 composition and Process parameters for the examples
| Item | Example 1 | Example 2 | Example 3 | Example 3 |
| PTFE（wt%） | 99 | 90 | 92 | 95 |
| n-BN（wt%） | 1 | 10 | 8 | 5 |
| Moulding pressure (MPa) | 130 | 140 | 130 | 120 |
| Holding time at 375 ℃h） | 2 | 2 | 2 | 5 |
Table 2 examples product performance testing
| Item | Example 1 | Example 2 | Example 3 | Example 4 |
| Tensile Strength (MPa) | 24.75 | 22.75 | 23.25 | 24.50 |
| Impact Strength (MPa) | 15.1 | 14.5 | 14.8 | 15.8 |
| Abrasion Property (g) | 0.0253 | 0.0059 | 0.0136 | 0.0150 |
| Coefficient of thermal conductivity (W.m)-1·K-1） | 0.4277 | 0.4478 | 0.4413 | 0.4436 |
Claims (7)
1. A PTFE/boron nitride composite material and a preparation method thereof are characterized in that: and obtaining a uniform mixture by adopting a liquid phase mixing method, and then performing cold pressing and sintering to obtain the composite material. The method comprises the following specific steps:
1) stripping of Boron Nitride (BN)
Treating hexagonal boron nitride powder with molten citric acid for 24h, washing with water to neutrality, filtering, and drying to obtain boron nitride nanosheet (n-BN);
2) liquid phase mixing of Polytetrafluoroethylene (PTFE) and boron nitride nanosheets (n-BN)
Respectively dispersing PTFE powder and boron nitride nanosheets (n-BN) in silicone oil to form stable emulsion, uniformly mixing, filtering, washing with dichloromethane, and drying to obtain mixed powder;
3) cold press forming and sintering
Placing the mixed powder into a die, and carrying out die pressing under certain pressure to obtain a blank; and then placing the shaped blank into a sintering furnace, and heating according to a certain program to sinter to finally obtain the PTFE/boron nitride composite material.
2. The PTFE/boron nitride composite of claim 1, wherein: the particle size of the boron nitride is 1-10 μm.
3. The PTFE/boron nitride composite of claim 1, wherein: the PTFE is suspended fine powder with the particle size of 20-80 mu m.
4. The PTFE/boron nitride composite of claim 1, wherein: in the step 1), the reaction temperature is 160-180 ℃.
5. The PTFE/boron nitride composite of claim 1, wherein: in the step 2), the mass fraction of n-BN is 1-10 wt%.
6. The PTFE/boron nitride composite of claim 1, wherein: in the step 3), the cold pressing pressure is 100-140 MPa.
7. The PTFE/boron nitride composite of claim 1, wherein: in the step 3), during the sintering process, the temperature control program is as follows:
I. the heating rate is 1.5 ℃/min, the target temperature is 130 ℃, and the temperature is kept for 1 h;
II, heating up at a rate of 1.4 ℃/min, keeping the target temperature at 250 ℃ for 1 h;
III, heating up at a rate of 1.1 ℃/min, keeping the temperature at the target temperature of 327 ℃ for 2 h;
IV, heating up at a rate of 1 ℃/min, keeping the temperature at 345 ℃ for 1 h;
v, the heating rate is 0.4 ℃/min, the target temperature is 375 ℃, and the temperature is kept for 1-5 h;
and VI, cooling along with the furnace.
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|---|---|---|---|---|
| CN113881172A (en) * | 2021-10-25 | 2022-01-04 | 西北橡胶塑料研究设计院有限公司 | Boron nitride modified polytetrafluoroethylene material and preparation method thereof |
| CN113929430A (en) * | 2021-10-26 | 2022-01-14 | 清华大学深圳国际研究生院 | Preparation method of pure or composite hexagonal boron nitride densified macroscopic body |
| CN113980307A (en) * | 2021-10-20 | 2022-01-28 | 清华大学深圳国际研究生院 | High-thermal-conductivity low-dielectric composite material and preparation method thereof |
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