CN104860680B - Wide-adaptability dual-mechanism self-lubricating bearing material and preparation method thereof - Google Patents
Wide-adaptability dual-mechanism self-lubricating bearing material and preparation method thereof Download PDFInfo
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Abstract
The invention provides a wide-adaptability dual-mechanism self-lubricating bearing material and a preparation method thereof, and relates to a bearing material. According to the method, ZrB2 nano powder, ZrO2 nano powder and CaF2 nano powder are used as raw materials to prepare the wide-adaptability dual-mechanism self-lubricating bearing material. The method comprises the following steps: firstly, cleaning the raw materials with a hydrofluoric acid water solution; then cleaning with deionized water and anhydrous ethanol, mixing the pre-treated ZrB2 nano powder, ZrO2 nano powder and CaF2 nano powder according to the weight percentage of 57.0-70.0% of ZrB2, 12.0-37.0% of ZrO2 and 6% of CaF2, stirring, dispersing and performing primary ball milling to obtain refined powder; adding the refined powder and the CaF2 nano powder into a container with deionized water, performing ultrasonic stirring and the like, performing secondary ball milling, and finally carrying out discharge plasma sintering to obtain the tool material. The prepared tool material adapts to high temperature and low temperature, and has characteristics of being fine and uniformly-distributed in granularity, high in hardness, bending strength and fracture toughness, excellent in s high-low temperature stability, and the like.
Description
Technical field
The present invention relates to a kind of material, specifically a kind of wide adaptation double-unit system self-lubricating bearing material and its preparation side
Method.
Background technology
Machinery manufacturing industry is occupied and its consequence in whole national economy, and bearing machining occupies in manufacturing industry
Leading position.Sliding bearing works sometimes under very exacting terms, and is in dusty circumstances so that common liq lubricates axle
Hold because its frictional behavior is limited it is impossible to adapt to the requirement of special operation condition.Self-lubricating technology bearing breaches dependence oils and fatss profit completely
Sliding limitation and achieve oil-free lubrication, self-lubricating material bearing technology is current lubrication technology development trend, mechanical strength
The high important focus being developed into tribological field with the good self-lubricating composite of tribological property.
There are some defects in current bearing material, due to operating mode such as temperature, load character, the load of bearing working
Species etc. is extremely complex, and dimensions is numerous, and how to select and to design suitable material according to different situations is complicated asking
Topic.Development high temperature, heavy duty, low speed, the self-lubricating bearing material containing under the complex working conditions such as lining and corrosivity are the task of top priority.
Content of the invention
It is an object of the present invention to provide a kind of wide adaptation double-unit system self-lubricating bearing material and preparation method thereof, the method combines
Add kollag and the double mechanism of in-situ oxidation reaction, the ZrB of powder2As matrix material and provide reaction in-situ
Self-lubricating mechanism, ZrO2For toughness reinforcing phase, CaF2For additive formula self-lubricating dispensing, prepare suitable self-lubricating bearing, and temperature is fitted
Answer the self-lubricating bearing material that scope is relatively wide.
A kind of width adapts to double-unit system self-lubricating bearing material, and the percent by volume of each raw material of this material is：ZrB257.0
~70.0%、ZrO212.0~37.0%、CaF26.0%.ZrB2Using nano powder, granularity is 40 ~ 50nm； ZrO2Using nano powder, grain
Spend for 10 ~ 20nm；CaF2Using nano powder, granularity is 150 ~ 155nm.The percent by volume of described each raw material is preferably：ZrB2
60.0%、ZrO234.0%、CaF26.0%.
A kind of wide adaptation double-unit system self-lubricating bearing material, comprises the following steps：
Step one, the pretreatment of raw material
Described ZrB2Nano powder, ZrO2Nano powder and CaF2Nano powder may be mixed with impurity in preparation and packaging process, is
Improve its purity, the hydrofluoric acid aqueous solution of employing is carried out.Because the granularity of nanopowder is less, activity is larger, for keeping away
Exempt from powder to be corroded by Fluohydric acid., the concentration of Fluohydric acid. should be suitably.Cleaning method is：Respectively by ZrB2Nano powder, ZrO2Nano powder
And CaF2Nano powder is placed in the hydrofluoric acid aqueous solution that concentration is 1.8wt%, then 80 ~ 100Hz ultrasound wave, 100 ~ 120r/min
Stir process 90 ~ 100min, stands 60 ~ 90min, pours out impurity of upper solution and floating etc., gained sediment add go from
Sub- water is washed, and standing 60 ~ 90min pours out upper solution again, adds deionized water to be washed again, until upper strata is molten
Till liquid pH value is more than 6.5, respectively obtain ZrB after pickling2Nano powder, ZrO2Nano powder and CaF2Nano powder；After gained pickling
ZrB2Nano powder, ZrO2Nano powder and CaF2Nano powder is separately added into absolute ethanol washing once, is then dried under vacuum to containing of water
Amount mass percent is 50%, adds absolute ethanol washing once again, then evacuation is preserved respectively, obtains pretreatment
ZrB afterwards2Nano powder, ZrO2Nano powder and CaF2Nano powder, standby；
Step 2, dispensing, stirring, dispersion and first time ball milling
According to ZrB2Percent by volume be 57.0 ~ 70.0%, ZrO2Percent by volume take respectively for 12.0 ~ 37.0% pre-
ZrB after process2Nano powder and ZrO2Nano powder, pours into equipped with ZrB2Nano powder and ZrO22 ~ 4 times of nano powder volume of mixture
In the container of deionized water, obtain mixture A；This container is combined with temperature sensor, can measure liquid in container at any time
Temperature；Container is placed in supersonic generator, 110 ~ 120Hz ultrasonic Treatment, 100 ~ 150r/min is carried out to it simultaneously and stir
Mix；During ultrasonic agitation, the temperature of mixture A is quickly increased to 110 DEG C, and keeps constant.Ultrasonic agitation 30 ~
After 40min, the mass ratio according to Polyethylene Glycol and mixture A is 1:90 taking polyethylene glycols, are added in mixture A, continue super
Sound stirs 10 ~ 20min, obtains mixture B；Gained mixture B is put in ball grinder, with dehydrated alcohol as medium, ball milling 180
~ 220h, is vacuum dried 22 ~ 26h under the conditions of 140 ~ 160 DEG C, sieves, and obtains refining powder, standby；
Step 3, second ball milling
The CaF that percent by volume according to above-mentioned steps two gained refinement powder is 94%, step one pretreatment obtains2Receive
The percent by volume of rice flour is 6%, takes the CaF that step 2 gained refinement powder and step one pretreatment obtain2Nano powder, pours into
Step 2 gained refines the CaF that powder and step one pretreatment obtain2The container of the deionized water that 6 ~ 8 times of nano powder cumulative volume
In, obtain mixture C；Described container is combined with temperature sensor, can measure the temperature of liquid in container at any time；Will be equipped with mixing
The container of compound C is placed in supersonic generator, 80 ~ 100Hz ultrasonic disperse, and it is carried out with 100 ~ 150r/min stirring simultaneously；
During ultrasonic agitation, mixture temperature is quickly increased to 100 DEG C, maintains this temperature, continue ultrasonic agitation 30 ~ 40min,
Mass ratio according to Polyethylene Glycol and mixture is 1:95 addition Polyethylene Glycol, then proceed to ultrasonic agitation and disperse 10 ~ 20min,
After ultrasonic agitation dispersion terminates, obtain mixture D；Gained mixture D is put in ball grinder, with dehydrated alcohol as medium, ball
Mill 180 ~ 220h, is vacuum dried 22 ~ 26h under the conditions of 140 ~ 160 DEG C, sieves, and obtains secondary ball milling refinement powder, standby；
Step 4：Discharge plasma sintering
Step 3 gained secondary ball milling refinement powder is loaded graphite jig, is placed in vacuum environment, then uniform pressurization
Carry out discharge plasma sintering, during sintering, during room temperature rises to 1700 DEG C, the adding to of ambient pressure even
45MPa, is 1750 DEG C, is incubated 10 ~ 25 min under the conditions of pressure 45MPa, then power-off naturally cools to room temperature in temperature afterwards,
Obtain wide adaptation double-unit system self-lubricating bearing material.
Ball grinder described in step 2 and step 3 is agate jar；
The method of ball milling described in step 2 and step 3 is wet type planetary ball mill.
Beneficial effect is：
1st, width of the present invention adapts to the preparation method of double-unit system self-lubricating bearing material, using the ZrB of powder2As matrix
Material simultaneously provides reaction in-situ self-lubricating mechanism, ZrO2For toughness reinforcing phase, CaF2For additive formula self-lubricating dispensing, and control each group
Point percent by volume be：ZrB260.0~80.0%、ZrO215.0~35.0%、CaF25.0%, introduce 15.0 ~ 35.0% ZrO2
Intensity and the toughness of composite, ZrB mainly can be improved2The ZrO that can also generate after oxidation2, make matrix phase ZrB2With new life
The ZrO becoming2, strengthen phase ZrO2Mutually interspersed, parcel, forms preferable framing structure, can form preferable transformation toughening effect
Really；Introduce 5.0% CaF2, mainly using this high-temperature lubricating material provides good self-lubricating in friction, utilizes simultaneously
ZrB2/ZrO2The support frame effect that ceramic matrix plays, and rely on three ball grinding techniques, by CaF2Kollag is embedded into
In continuous ceramic skeleton, can separate out in slow cutting or friction, play the effect of self-lubricating and antifriction.
2nd, the present invention provides the wide preparation method adapting to double-unit system self-lubricating bearing material, by ZrB2Add in matrix
ZrO2Powder and CaF2Powder, and control respective volume fraction, using vacuum environment, the discharge plasma sintering of uniform pressurization
（SPS）Technique, this sintering process can effectively reduce the sintering temperature compared with hard-to-sinter boride composite, thus obtaining densification
The material of Du Genggao；Under this process conditions, the wide of preparation adapts to double-unit system self-lubricating bearing material, is suitable for high/low temperature, has
Granularity is tiny and be evenly distributed, high rigidity, high-flexural strength, high-fracture toughness, good height temperature stability the features such as, be suitable for
In making, higher bearing is required to high temperature and wearability.
Brief description
Fig. 1 is that the percent by volume of each component in raw material is：ZrB255.0%、ZrO240.0%、CaF25.0%, other
Part according to width of the present invention adapt to double-unit system self-lubricating bearing material preparation method in constant, prepared material is at 700 °C
Picture after lower fretting wear；
Fig. 2 is wide adaptation double-unit system self-lubricating bearing material picture after 700 °C of lower fretting wears of embodiment two preparation；
Fig. 3 is that the percent by volume of each component in raw material is：ZrB285.0%、ZrO210.0%、CaF25.0%, other
Part adapts to double-unit system self-lubricating bearing material picture after 700 °C of lower fretting wears according to the present invention is wide；
Fig. 4 is friction temperature and coefficient of friction graph of a relation in high temperature friction and wear experiment；
Fig. 5 is wide adaptation self lubrication mechanism-friction incipient stage in friction process for the double-unit system self-lubricating bearing material
Schematic diagram；
Fig. 6 is wide adaptation self lubrication mechanism-ZrB in friction process for the double-unit system self-lubricating bearing material2、CaF2Granule
Gradually separate out schematic diagram；
Fig. 7 is wide adaptation self lubrication mechanism-B in friction process for the double-unit system self-lubricating bearing material2O3, ZrO2,
CaF2Lubricating film drags in friction surface and covers schematic diagram；
Fig. 8 is the wide shape adapting to self lubrication mechanism-self-lubricating film in friction process for the double-unit system self-lubricating bearing material
Become schematic diagram；
Fig. 9 be wide adapt to double-unit system self-lubricating bearing material under 700 C in the air aoxidize 2 hours after remaining bending resistance strong
Degree figure；
Figure 10 be wide adaptation double-unit system self-lubricating bearing material under 700 C after in the air aoxidizes 2 hours remaining fracture tough
Property figure.
Specific embodiment
A kind of width adapts to double-unit system self-lubricating bearing material, and the percent by volume of each raw material of this material is：ZrB257.0
~70.0%、ZrO212.0~37.0%、CaF26.0%.ZrB2Using nano powder, granularity is 40 ~ 50nm； ZrO2Using nano powder, grain
Spend for 10 ~ 20nm；CaF2Using nano powder, granularity is 150 ~ 155nm.The percent by volume of described each raw material is preferably：ZrB2
60.0%、ZrO234.0%、CaF26.0%.
A kind of wide adaptation double-unit system self-lubricating bearing material, comprises the following steps：
Step one, the pretreatment of raw material
Described ZrB2Nano powder, ZrO2Nano powder and CaF2Nano powder may be mixed with impurity in preparation and packaging process, is
Improve its purity, the hydrofluoric acid aqueous solution of employing is carried out.Because the granularity of nanopowder is less, activity is larger, for keeping away
Exempt from powder to be corroded by Fluohydric acid., the concentration of Fluohydric acid. should be suitably.Cleaning method is：Respectively by ZrB2Nano powder, ZrO2Nano powder
And CaF2Nano powder is placed in the hydrofluoric acid aqueous solution that concentration is 1.8wt%, then 80 ~ 100Hz ultrasound wave, 100 ~ 120r/min
Stir process 90 ~ 100min, stands 60 ~ 90min, pours out impurity of upper solution and floating etc., gained sediment add go from
Sub- water is washed, and standing 60 ~ 90min pours out upper solution again, adds deionized water to be washed again, until upper strata is molten
Till liquid pH value is more than 6.5, respectively obtain ZrB after pickling2Nano powder, ZrO2Nano powder and CaF2Nano powder；After gained pickling
ZrB2Nano powder, ZrO2Nano powder and CaF2Nano powder is separately added into absolute ethanol washing once, is then dried under vacuum to containing of water
Amount mass percent is 50%, adds absolute ethanol washing once again, then evacuation is preserved respectively, obtains pretreatment
ZrB afterwards2Nano powder, ZrO2Nano powder and CaF2Nano powder, standby；
Step 2, dispensing, stirring, dispersion and first time ball milling
According to ZrB2Percent by volume be 57.0 ~ 70.0%, ZrO2Percent by volume take respectively for 12.0 ~ 37.0% pre-
ZrB after process2Nano powder and ZrO2Nano powder, pours into equipped with ZrB2Nano powder and ZrO22 ~ 4 times of nano powder volume of mixture
In the container of deionized water, obtain mixture A；This container is combined with temperature sensor, can measure liquid in container at any time
Temperature；Container is placed in supersonic generator, 110 ~ 120Hz ultrasonic Treatment, 100 ~ 150r/min is carried out to it simultaneously and stir
Mix；During ultrasonic agitation, the temperature of mixture A is quickly increased to 110 DEG C, and keeps constant.Ultrasonic agitation 30 ~
After 40min, the mass ratio according to Polyethylene Glycol and mixture A is 1:90 taking polyethylene glycols, are added in mixture A, continue super
Sound stirs 10 ~ 20min, obtains mixture B；Gained mixture B is put in ball grinder, with dehydrated alcohol as medium, ball milling 180
~ 220h, is vacuum dried 22 ~ 26h under the conditions of 140 ~ 160 DEG C, sieves, and obtains refining powder, standby；
Step 3, second ball milling
The CaF that percent by volume according to above-mentioned steps two gained refinement powder is 94%, step one pretreatment obtains2Receive
The percent by volume of rice flour is 6%, takes the CaF that step 2 gained refinement powder and step one pretreatment obtain2Nano powder, pours into
Step 2 gained refines the CaF that powder and step one pretreatment obtain2The container of the deionized water that 6 ~ 8 times of nano powder cumulative volume
In, obtain mixture C；Described container is combined with temperature sensor, can measure the temperature of liquid in container at any time；Will be equipped with mixing
The container of compound C is placed in supersonic generator, 80 ~ 100Hz ultrasonic disperse, and it is carried out with 100 ~ 150r/min stirring simultaneously；
During ultrasonic agitation, mixture temperature is quickly increased to 100 DEG C, maintains this temperature, continue ultrasonic agitation 30 ~ 40min,
Mass ratio according to Polyethylene Glycol and mixture is 1:95 addition Polyethylene Glycol, then proceed to ultrasonic agitation and disperse 10 ~ 20min,
After ultrasonic agitation dispersion terminates, obtain mixture D；Gained mixture D is put in ball grinder, with dehydrated alcohol as medium, ball
Mill 180 ~ 220h, is vacuum dried 22 ~ 26h under the conditions of 140 ~ 160 DEG C, sieves, and obtains secondary ball milling refinement powder, standby；
Step 4：Discharge plasma sintering
Step 3 gained secondary ball milling refinement powder is loaded graphite jig, is placed in vacuum environment, then uniform pressurization
Carry out discharge plasma sintering, during sintering, during room temperature rises to 1700 DEG C, the adding to of ambient pressure even
45MPa, is 1750 DEG C, is incubated 10 ~ 25 min under the conditions of pressure 45MPa, then power-off naturally cools to room temperature in temperature afterwards,
Obtain wide adaptation double-unit system self-lubricating bearing material.
Ball grinder described in step 2 and step 3 is agate jar；
The method of ball milling described in step 2 and step 3 is wet type planetary ball mill.
Embodiment 1
A kind of width adapts to double-unit system self-lubricating bearing material, and the percent by volume of each raw material of this material is：ZrB2
57.0%、ZrO237.0%、CaF26.0%.ZrB2Using nano powder, granularity is 40nm； ZrO2Using nano powder, granularity is 10nm；
CaF2Using nano powder, granularity is 150nm.
A kind of wide adaptation double-unit system self-lubricating bearing material, comprises the following steps：
Step one, the pretreatment of raw material
Described ZrB2Nano powder, ZrO2Nano powder and CaF2Nano powder may be mixed with impurity in preparation and packaging process, is
Improve its purity, the hydrofluoric acid aqueous solution of employing is carried out.Because the granularity of nanopowder is less, activity is larger, for keeping away
Exempt from powder to be corroded by Fluohydric acid., the concentration of Fluohydric acid. should be suitably.Cleaning method is：Respectively by ZrB2Nano powder, ZrO2Nano powder
And CaF2Nano powder is placed in the hydrofluoric acid aqueous solution that concentration is 1.8wt%, then 80Hz ultrasound wave, 100r/min stir process
90min, stands 60min, pours out impurity of upper solution and floating etc., and gained sediment adds deionized water to be washed, quiet
Put 60min and pour out upper solution again, add deionized water to be washed again, till upper solution pH value is more than 6.5,
Respectively obtain ZrB after pickling2Nano powder, ZrO2Nano powder and CaF2Nano powder；By ZrB after gained pickling2Nano powder, ZrO2Nanometer
Powder and CaF2Nano powder is separately added into absolute ethanol washing once, and the content mass percent being then dried under vacuum to water is 50%,
Add absolute ethanol washing once again, then evacuation is preserved respectively, obtains ZrB after pretreatment2Nano powder, ZrO2Receive
Rice flour and CaF2Nano powder, standby；
Step 2, dispensing, stirring, dispersion and first time ball milling
According to ZrB2Percent by volume be 57.0%, ZrO2Percent by volume take respectively for 37.0% pretreated
ZrB2Nano powder and ZrO2Nano powder, pours into equipped with ZrB2Nano powder and ZrO2The deionized water that 2 times of nano powder volume of mixture
In container, obtain mixture A；This container is combined with temperature sensor, can measure the temperature of liquid in container at any time；By container
It is placed in supersonic generator, 110 ~ 120Hz ultrasonic Treatment, it is carried out with 100 ~ 150r/min stirring simultaneously；Stir ultrasonic
During mixing, the temperature of mixture A is quickly increased to 110 DEG C, and keeps constant.After ultrasonic agitation 30 ~ 40min, according to poly-
The mass ratio of ethylene glycol and mixture A is 1:90 taking polyethylene glycols, are added in mixture A, continue ultrasonic agitation 10 ~ 20min,
Obtain mixture B；Gained mixture B is put in ball grinder, with dehydrated alcohol as medium, ball milling 180 ~ 220h, 140 ~ 160
It is vacuum dried 22 ~ 26h under the conditions of DEG C, sieves, obtain refining powder, standby；
Step 3, second ball milling
The CaF that percent by volume according to above-mentioned steps two gained refinement powder is 94%, step one pretreatment obtains2Receive
The percent by volume of rice flour is 6%, takes the CaF that step 2 gained refinement powder and step one pretreatment obtain2Nano powder, pours into
Step 2 gained refines the CaF that powder and step one pretreatment obtain2The container of the deionized water that 6 ~ 8 times of nano powder cumulative volume
In, obtain mixture C；Described container is combined with temperature sensor, can measure the temperature of liquid in container at any time；Will be equipped with mixing
The container of compound C is placed in supersonic generator, 80 ~ 100Hz ultrasonic disperse, carries out 100r/min stirring to it simultaneously；Super
In sound whipping process, mixture temperature is quickly increased to 100 DEG C, maintains this temperature, continue ultrasonic agitation 30 ~ 40min, according to
The mass ratio of Polyethylene Glycol and mixture is 1:95 addition Polyethylene Glycol, then proceed to ultrasonic agitation dispersion 10min, ultrasonic agitation
After dispersion terminates, obtain mixture D；Gained mixture D is put in agate jar, with dehydrated alcohol as medium, wet type row
Celestial body grinds 180h, is vacuum dried 22h, sieves under the conditions of 140 DEG C, obtains secondary ball milling refinement powder, standby；
Step 4：Discharge plasma sintering
Step 3 gained secondary ball milling refinement powder is loaded graphite jig, is placed in vacuum environment, then uniform pressurization
Carry out discharge plasma sintering, during sintering, during room temperature rises to 1700 DEG C, the adding to of ambient pressure even
45MPa, is 1750 DEG C, is incubated 10 min under the conditions of pressure 45MPa, then power-off naturally cools to room temperature, that is, in temperature afterwards
Obtain wide adaptation double-unit system self-lubricating bearing material.
Embodiment 2
A kind of width adapts to double-unit system self-lubricating bearing material, and the percent by volume of each raw material of this material is：ZrB2
60.0%、ZrO234.0%、CaF26.0%.ZrB2Using nano powder, granularity is 45nm； ZrO2Using nano powder, granularity is 15nm；
CaF2Using nano powder, granularity is 152nm.
A kind of wide adaptation double-unit system self-lubricating bearing material, comprises the following steps：
Step one, the pretreatment of raw material
Described ZrB2Nano powder, ZrO2Nano powder and CaF2Nano powder may be mixed with impurity in preparation and packaging process, is
Improve its purity, the hydrofluoric acid aqueous solution of employing is carried out.Because the granularity of nanopowder is less, activity is larger, for keeping away
Exempt from powder to be corroded by Fluohydric acid., the concentration of Fluohydric acid. should be suitably.Cleaning method is：Respectively by ZrB2Nano powder, ZrO2Nano powder
And CaF2Nano powder is placed in the hydrofluoric acid aqueous solution that concentration is 1.8wt%, then 90Hz ultrasound wave, 110r/min stir process
95min, stands 80min, pours out impurity of upper solution and floating etc., and gained sediment adds deionized water to be washed, quiet
Put 80min and pour out upper solution again, add deionized water to be washed again, till upper solution pH value is more than 6.5,
Respectively obtain ZrB after pickling2Nano powder, ZrO2Nano powder and CaF2Nano powder；By ZrB after gained pickling2Nano powder, ZrO2Nanometer
Powder and CaF2Nano powder is separately added into absolute ethanol washing once, and the content mass percent being then dried under vacuum to water is 50%,
Add absolute ethanol washing once again, then evacuation is preserved respectively, obtains ZrB after pretreatment2Nano powder, ZrO2Receive
Rice flour and CaF2Nano powder, standby；
Step 2, dispensing, stirring, dispersion and first time ball milling
According to ZrB2Percent by volume be 60.0%, ZrO2Percent by volume take respectively for 34.0% pretreated
ZrB2Nano powder and ZrO2Nano powder, pours into equipped with ZrB2Nano powder and ZrO2The deionized water that 3 times of nano powder volume of mixture
In container, obtain mixture A；This container is combined with temperature sensor, can measure the temperature of liquid in container at any time；By container
It is placed in supersonic generator, 110Hz ultrasonic Treatment, 100r/min stirring is carried out to it simultaneously；During ultrasonic agitation,
The temperature of mixture A is quickly increased to 110 DEG C, and keeps constant.After ultrasonic agitation 30min, according to Polyethylene Glycol and mixing
The mass ratio of thing A is 1:90 taking polyethylene glycols, are added in mixture A, continue ultrasonic agitation 10min, obtain mixture B；Will
Gained mixture B puts in ball grinder, with dehydrated alcohol as medium, ball milling 200h, and it is vacuum dried 22h, mistake under the conditions of 140 DEG C
Sieve, obtains refining powder, standby；
Step 3, second ball milling
The CaF that percent by volume according to above-mentioned steps two gained refinement powder is 94%, step one pretreatment obtains2Receive
The percent by volume of rice flour is 6%, takes the CaF that step 2 gained refinement powder and step one pretreatment obtain2Nano powder, pours into
Step 2 gained refines the CaF that powder and step one pretreatment obtain2In the container of the deionized water that 7 times of nano powder cumulative volume,
Obtain mixture C；Described container is provided with temperature sensor, can measure the temperature of liquid in container at any time；Will be equipped with mixture C
Container be placed in supersonic generator, 90Hz ultrasonic disperse, 120r/min stirring is carried out to it simultaneously；In ultrasonic agitation process
In, mixture temperature is quickly increased to 100 DEG C, maintains this temperature, continue ultrasonic agitation 35min, according to Polyethylene Glycol and mixed
The mass ratio of compound is 1:95 addition Polyethylene Glycol, then proceed to ultrasonic agitation dispersion 15min, after ultrasonic agitation dispersion terminates,
Obtain mixture D；Gained mixture D is put in agate jar, with dehydrated alcohol as medium, wet type planetary ball mill 200h,
It is vacuum dried 24h under the conditions of 150 DEG C, sieves, obtain secondary ball milling refinement powder, standby；
Step 4：Discharge plasma sintering
Step 3 gained secondary ball milling refinement powder is loaded graphite jig, is placed in vacuum environment, then uniform pressurization
Carry out discharge plasma sintering, during sintering, during room temperature rises to 1700 DEG C, the adding to of ambient pressure even
45MPa, is 1750 DEG C, is incubated 20min under the conditions of pressure 45MPa, then power-off naturally cools to room temperature, obtains final product in temperature afterwards
Adapt to double-unit system self-lubricating bearing material to wide.
Fig. 2 show the wide adaptation double-unit system self-lubricating bearing material of embodiment two preparation after 700 °C of lower fretting wears
Picture.It is Al to the material that rubs2O3.Contrast Fig. 1, from form, the wide of embodiment two preparation adapts to double-unit system self-lubricating bearing material
Material has preferable self-lubricating performance after to mill, and the distribution of self-lubricating film is more uniform, surface particles and seriously takes off
The phenomenon falling, the overall better performances of material.
Embodiment 3
A kind of width adapts to double-unit system self-lubricating bearing material, and the percent by volume of each raw material of this material is：ZrB2
70.0%、ZrO224.0%、CaF26.0%.ZrB2Using nano powder, granularity is 50nm； ZrO2Using nano powder, granularity is 20nm；
CaF2Using nano powder, granularity is 155nm.
A kind of wide adaptation double-unit system self-lubricating bearing material, comprises the following steps：
Step one, the pretreatment of raw material
Described ZrB2Nano powder, ZrO2Nano powder and CaF2Nano powder may be mixed with impurity in preparation and packaging process, is
Improve its purity, the hydrofluoric acid aqueous solution of employing is carried out.Because the granularity of nanopowder is less, activity is larger, for keeping away
Exempt from powder to be corroded by Fluohydric acid., the concentration of Fluohydric acid. should be suitably.Cleaning method is：Respectively by ZrB2Nano powder, ZrO2Nano powder
And CaF2Nano powder is placed in the hydrofluoric acid aqueous solution that concentration is 1.8wt%, then 100Hz ultrasound wave, 120r/min stir process
100min, stands 60 ~ 90min, pours out impurity of upper solution and floating etc., and gained sediment adds deionized water to be washed
Wash, standing 90min pours out upper solution again, add deionized water to be washed again, until upper solution pH value is more than 6.5
Till, respectively obtain ZrB after pickling2Nano powder, ZrO2Nano powder and CaF2Nano powder；By ZrB after gained pickling2Nano powder,
ZrO2Nano powder and CaF2Nano powder is separately added into absolute ethanol washing once, is then dried under vacuum to the content percent mass of water
Ratio for 50%, adds absolute ethanol washing once, then evacuation is preserved respectively, obtains ZrB after pretreatment again2Nanometer
Powder, ZrO2Nano powder and CaF2Nano powder, standby；
Step 2, dispensing, stirring, dispersion and first time ball milling
According to ZrB2Percent by volume be 70.0%, ZrO2Percent by volume take respectively for 37.0% pretreated
ZrB2Nano powder and ZrO2Nano powder, pours into equipped with ZrB2Nano powder and ZrO2The deionized water that 2 ~ 4 times of nano powder volume of mixture
Container in, obtain mixture A；This container is combined with temperature sensor, can measure the temperature of liquid in container at any time；To hold
Device is placed in supersonic generator, 110 ~ 120Hz ultrasonic Treatment, carries out 150r/min stirring to it simultaneously；In ultrasonic agitation
During, the temperature of mixture A is quickly increased to 110 DEG C, and keeps constant.After ultrasonic agitation 40min, according to Polyethylene Glycol
Mass ratio with mixture A is 1:90 taking polyethylene glycols, are added in mixture A, continue ultrasonic agitation 20min, are mixed
Thing B；Gained mixture B is put in ball grinder, with dehydrated alcohol as medium, ball milling 220h, it is vacuum dried under the conditions of 160 DEG C
26h, sieves, and obtains refining powder, standby；
Step 3, second ball milling
The CaF that percent by volume according to above-mentioned steps two gained refinement powder is 94%, step one pretreatment obtains2Receive
The percent by volume of rice flour is 6%, takes the CaF that step 2 gained refinement powder and step one pretreatment obtain2Nano powder, pours into
Step 2 gained refines the CaF that powder and step one pretreatment obtain2In the container of the deionized water that 8 times of nano powder cumulative volume,
Obtain mixture C；Described container is combined with temperature sensor, can measure the temperature of liquid in container at any time；Will be equipped with mixing
The container of thing C is placed in supersonic generator, 100Hz ultrasonic disperse, carries out 150r/min stirring to it simultaneously；Stir ultrasonic
During mixing, mixture temperature is quickly increased to 100 DEG C, maintains this temperature, continue ultrasonic agitation 40min, according to poly- second two
The mass ratio of alcohol and mixture is 1:95 addition Polyethylene Glycol, then proceed to ultrasonic agitation dispersion 20min, ultrasonic agitation dispersion knot
Shu Hou, obtains mixture D；Gained mixture D is put in agate jar, with dehydrated alcohol as medium, wet type planetary ball mill
220h, is vacuum dried 26h under the conditions of 160 DEG C, sieves, and obtains secondary ball milling refinement powder, standby；
Step 4：Discharge plasma sintering
Step 3 gained secondary ball milling refinement powder is loaded graphite jig, is placed in vacuum environment, then uniform pressurization
Carry out discharge plasma sintering, during sintering, during room temperature rises to 1700 DEG C, the adding to of ambient pressure even
45MPa, is 1750 DEG C, is incubated 10 ~ 25 min under the conditions of pressure 45MPa, then power-off naturally cools to room temperature in temperature afterwards,
Obtain wide adaptation double-unit system self-lubricating bearing material.
Width of the present invention adapts to self lubrication mechanism in friction process for the double-unit system self-lubricating bearing material
As shown in Fig. 5 to Fig. 8, show for the wide self lubrication mechanism in friction process for the double-unit system self-lubricating bearing material that adapts to
It is intended to, Fig. 5 represents the friction incipient stage, Fig. 6 represents ZrB2、CaF2Granule gradually separates out, and Fig. 7 represents B2O3, CaF2, ZrO2Profit
Lubrication prescription drags in friction surface and covers, and Fig. 8 represents the formation of self-lubricating film.As shown in figure 5, when self-lubricating material is cut or rubs
When, a large amount of frictional heats can be produced between friction pair, be in self-lubricating material top layer and acted on by frictional heat and compressive stress, TiB2、
ZrB2Granule gradually separates out；As shown in fig. 6, in the presence of High Temperature High Pressure and oxygen, being susceptible to friction chemical reaction, in material
Material Surface Creation has the ZrB of lubrication2, CaF2, ZrO2Lubricating film；As shown in fig. 7, after friction, due to solid profit
The hardness of lubrication prescription and shear strength are relatively low, thus separate out surface kollag under rubbing action it is easy to be overlayed on by dragging
Friction surface, when a large amount of solid lubricant particles are dragged and cover, just defines lubricating film in friction surface；As shown in figure 8, no matter
It is to form complete lubricating film between rubbing surface, or forming part lubricating film all can play the effect of antifriction.
The present invention utilizes the wide adaptation double-unit system self-lubricating bearing material prepared by zirconium boride, zirconium oxide, calcium fluoride, in height
Kollag under warm rubbing action and the double mechanism self-lubricating of in-situ oxidation reaction, generate in material surface and have lubrication
The reaction film of effect, thus realizing self-lubricating, correlation technique can be prepared one kind and be not only suitable for high-speed cutting and in low temperature
Also unrestricted adapt to double-unit system self-lubricating bearing material to wide.
Related experiment
1st, width of the present invention adapts to the experiment of double-unit system self-lubricating bearing material high temperature friction and wear：
Friction-wear test is carried out in UMT-2 Multifunctional friction experimental machine (U.S., CETR company).This frictional testing machine
, in 0 ~ 200N, precision is up to 10mN for the working range of sensor；Horizontally and vertically displacement accuracy is 0.1mm/s；The speed of mainshaft is 0
~ 5000rev/min, precision is up to 0.1 rev/min；At 0 ~ 1000 DEG C, precision is 0.1 DEG C to the working range of heating chamber.Infrared
System for detecting temperature precision is 0.5 DEG C.The secondary form of joining of friction selects ball-disk friction-type.To the material that rubs：Al2O3.Experiment is respectively
From four groups of materials, one group is pure ZrB2,Two groups is that the percent by volume of raw material is：ZrB255.0%、ZrO240.0%、CaF2
5.0%, other composition preparation methoies are identical with the present invention；Three groups is that width of the present invention adapts to double-unit system self-lubricating bearing material；Four groups
It is that the percent by volume of raw material is：ZrB265.0%、ZrO230.0%、CaF25.0%, other composition preparation methoies and the present invention
Identical；Coefficient of friction and friction temperature graph of a relation in the experiment of its result high temperature friction and wear as shown in Figure 4.Can from figure
Go out, general ZrB2There is reaction in-situ at 500 ~ 700 DEG C, form reaction in-situ self-lubricating.But when 500 DEG C, pure ZrB2With
Al2O3During to rubbing, due to can not there is self-lubricating, coefficient of friction has reached 0.65, and width of the present invention adapts to double-unit system self-lubricating bearing
Material, when below 500 DEG C, the kollag CaF of interpolation2Lubricating film can be generated, therefore coefficient of friction is significantly lower than pure
ZrB2.And width of the present invention adapts to double-unit system self-lubricating bearing material, after temperature is higher than 700 DEG C, reaction in-situ all can occur.From
In figure can be seen that the material of the present invention is higher than 700 DEG C in temperature, and all can show preferable self lubricity during less than 500 DEG C
Can, it is preferable cutter material；
2nd, the present invention is wide adapts to double-unit system self-lubricating bearing material in the air oxidation experiment under 700 C：
Material in this experiment, other compositions are all identical with the present invention with preparation method, ZrO2Percent by volume contain
Amount is different；As shown in Fig. 9 and Figure 10, this figure is respectively different ZrO to experimental result2The material of content in the air oxygen under 700 C
Remaining bending strength figure after changing 2 hours and remaining fracture toughness figure；It can be seen that working as ZrB2For percent by volume
Content is that the residual mechanical properties after oxidation when 30% are best, than（ZrB295vol.%+ CaF25vol.%）Ceramic material residual
Remaining bending strength improves 88.3%, and remaining fracture toughness improves 96.9%.It is demonstrated experimentally that width of the present invention adapts to double-unit system from profit
Plain besring material has stronger bending strength and remaining fracture toughness.
3rd, when in the preparation method of width adaptation double-unit system self-lubricating bearing material of the present invention, raw material component ratio changes
Experiment：
（1）, when the percent by volume of component each in raw material be：ZrB255.0%、ZrO240.0%、CaF25.0%, other
Condition adapts to constant, the prepared material in the preparation method of double-unit system self-lubricating bearing material according to width of the present invention, carries out
In 700 °C of lower frictional wear experiments, it is Al to the material that rubs2O3；Fig. 1 is experimental result；According to EDX figure and X-ray diffraction
Black region in Fig. 1 is ZrO2, canescence region is ZrB2, white reflection region is CaF2.From figure 1 it appears that high temperature
Between crystal grain after frictional wear experiment, the combination degree at interface has weakened, and there is the phenomenon of particle detachment on surface, from form
See and do not show good double-unit system self-lubricating effect.It is primarily due to work as ZrO2Content more than 35% when, ZrO2Material itself
The relatively low feature of hardness just shows although ZrO2There is the effect of transformation toughening, but the bulk strength of material is in high temperature
Also suffer from after fretting wear necessarily affecting.
（2）, when the percent by volume of component each in raw material be：ZrB285.0%、ZrO210.0%、CaF25.0%, other
Condition adapts to constant, the prepared material in the preparation method of double-unit system self-lubricating bearing material according to width of the present invention, carries out
In 700 °C of lower frictional wear experiments, it is Al to the material that rubs2O3；Fig. 3 is experimental result；Contrast Fig. 2, prepared material passes through
More serious to the abrasion dropping situations of material after rubbing, the consistency of material is moistened certainly than the wide adaptation double-unit system prepared by the present invention
Plain besring material is less better, does not show good double-unit system self-lubricating effect.Work as ZrB2Content more than 80% when, ZrB2
The more difficult feature of material densification itself just shows the ZrO although a small amount of2There is the effect of transformation toughening, but material
Bulk strength also suffer from necessarily affecting after high temperature friction and wear.
Claims (6)
1. a kind of wide adapt to double-unit system self-lubricating bearing material it is characterised in that：The percent by volume of each raw material of this material is：
ZrB257.0~70.0%、ZrO212.0~37.0%、CaF26.0%；ZrB2Using nano powder, granularity is 40 ~ 50nm； ZrO2Using
Nano powder, granularity is 10 ~ 20nm；CaF2Using nano powder, granularity is 150 ~ 155nm.
2. as claimed in claim 1 a kind of wide adapt to double-unit system self-lubricating bearing material it is characterised in that：Described each raw material
Percent by volume is：ZrB260.0%、ZrO234.0%、CaF26.0%.
3. a kind of width adapts to the preparation method of double-unit system self-lubricating bearing material as claimed in claim 1 or 2, and its feature exists
In：Comprise the following steps：
Step one, the pretreatment of raw material
Respectively by ZrB2Nano powder, ZrO2Nano powder and CaF2Nano powder is placed in the hydrofluoric acid aqueous solution that concentration is 1.8wt%, so
80 ~ 100Hz ultrasound wave, 100 ~ 120r/min stir process 90 ~ 100min afterwards, stands 60 ~ 90min, pours out upper solution and drift
Floating impurity, gained sediment adds deionized water to be washed, and standing 60 ~ 90min pours out upper solution again, adds again
Deionized water is washed, and till upper solution pH value is more than 6.5, respectively obtains ZrB after pickling2Nano powder, ZrO2Nanometer
Powder and CaF2Nano powder；By ZrB after gained pickling2Nano powder, ZrO2Nano powder and CaF2Nano powder is separately added into dehydrated alcohol and washes
Wash, obtain ZrB after pretreatment2Nano powder, ZrO2Nano powder and CaF2Nano powder, standby；
Step 2, dispensing, stirring, dispersion and first time ball milling
According to ZrB2Percent by volume be 57.0 ~ 70.0%, ZrO2Percent by volume take pretreatment respectively for 12.0 ~ 37.0%
ZrB afterwards2Nano powder and ZrO2Nano powder, pours into equipped with ZrB2Nano powder and ZrO22 ~ 4 times of nano powder volume of mixture go from
Sub- water and be provided with the container of temperature sensor, obtains mixture A；The container that will be equipped with mixture A is placed in supersonic generator
In, 110 ~ 120Hz ultrasonic Treatment, it is carried out with 100 ~ 150r/min stirring simultaneously；During ultrasonic agitation, by mixture
The temperature of A is increased to 110 DEG C, maintains this temperature, ultrasonic agitation 30 ~ 40min, according to the mass ratio of Polyethylene Glycol and mixture A
For 1:90 taking polyethylene glycols, are added in mixture A, continue ultrasonic agitation 10 ~ 20min, obtain mixture B；Gained is mixed
Thing B puts in ball grinder, with dehydrated alcohol as medium, ball milling 180 ~ 220h, under the conditions of 140 ~ 160 DEG C vacuum drying 22 ~
26h, sieves, and obtains refining powder, standby；
Step 3, second ball milling
The CaF that percent by volume according to above-mentioned steps two gained refinement powder is 94%, step one pretreatment obtains2Nano powder
Percent by volume is 6%, takes the CaF that step 2 gained refinement powder and step one pretreatment obtain2Nano powder, pours step 2 into
Gained refines the CaF that powder and step one pretreatment obtain2In the container of the deionized water that 6 ~ 8 times of nano powder cumulative volume, obtain
Mixture C；Described container is provided with temperature sensor；The container that will be equipped with mixture C is placed in supersonic generator, 80 ~ 100Hz
Ultrasonic Treatment, carries out 100 ~ 150r/min stirring simultaneously to it；During ultrasonic agitation, mixture temperature is increased to
100 DEG C, maintain this temperature, continue ultrasonic agitation 30 ~ 40min, the mass ratio according to Polyethylene Glycol and mixture is 1:95 additions
Polyethylene Glycol, then proceedes to ultrasonic agitation and disperses 10 ~ 20min, after ultrasonic agitation dispersion terminates, obtain mixture D；Gained is mixed
Compound D puts in ball grinder, with dehydrated alcohol as medium, ball milling 180 ~ 220h, under the conditions of 140 ~ 160 DEG C vacuum drying 22 ~
26h, sieves, and obtains secondary ball milling refinement powder, standby；
Step 4：Discharge plasma sintering
Step 3 gained secondary ball milling refinement powder is loaded graphite jig, is placed in vacuum environment, then uniform pressurization is carried out
Discharge plasma sintering, during sintering, during room temperature rises to 1700 DEG C, ambient pressure even add to 45MPa,
It is 1750 DEG C, is incubated 10 ~ 25 min under the conditions of pressure 45MPa, then power-off naturally cools to room temperature, that is, obtains in temperature afterwards
Wide adaptation double-unit system self-lubricating bearing material.
4. the wide preparation method adapting to double-unit system self-lubricating bearing material as claimed in claim 3 it is characterised in that：Step 2 and
Ball grinder described in step 3 is agate jar.
5. the wide preparation method adapting to double-unit system self-lubricating bearing material as claimed in claim 3 it is characterised in that：Step 2 and
The method of ball milling described in step 3 is wet type planetary ball mill.
6. the wide preparation method adapting to double-unit system self-lubricating bearing material as claimed in claim 3 it is characterised in that：Described by institute
Obtain ZrB after pickling2Nano powder, ZrO2Nano powder and CaF2Nano powder using the method that dehydrated alcohol is washed is：It is separately added into
Once, the content mass percent being then dried under vacuum to water is 50% to absolute ethanol washing, adds absolute ethanol washing one again
Secondary, then evacuation is preserved respectively, standby.
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| CN101913876A (en) * | 2010-07-01 | 2010-12-15 | 山东大学 | Method for preparing zirconium boride-tungsten titanium carbide self-lubricating composite ceramic material |
| CN102899550A (en) * | 2012-09-24 | 2013-01-30 | 江苏利达不锈钢有限公司 | High temperature resistant self-lubricating bearing material and preparation method thereof |
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| CN101117608A (en) * | 2007-07-21 | 2008-02-06 | 李文远 | Micro-powder antifriction self-repair lubricating material and preparation method and using method thereof |
| CN101913876A (en) * | 2010-07-01 | 2010-12-15 | 山东大学 | Method for preparing zirconium boride-tungsten titanium carbide self-lubricating composite ceramic material |
| CN102899550A (en) * | 2012-09-24 | 2013-01-30 | 江苏利达不锈钢有限公司 | High temperature resistant self-lubricating bearing material and preparation method thereof |
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