CN104860680A - 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 preparation method thereof.
Background technology
Machinery manufacturing industry is occupied and consequence in whole national economy, and bearing machining dominate in production.Sliding surface bearing works sometimes under very exacting terms, and is in dusty circumstances, common liq lubricating bearings limit because of its rubbing characteristics, can not adapt to the requirement of special operation condition.Self-lubricating technology bearing breaches completely and relies on the limitation of grease lubrication and achieve oil-free lubricatoin, self-lubricating material bearing technology is current lubrication technology development trend, and the exploitation of the self-lubricating composite that mechanical strength is high and tribological property is good becomes the important focus of tribological field.
There are some defects in current bearing materials, because operating mode such as temperature, load character, the load categories etc. of bearing working are very complicated, dimensions is numerous, and how to select according to different situations and to design suitable material is a complicated problem.Development high temperature, heavy duty, low speed, be the task of top priority containing the self-lubricating bearing material under lining and the complex working condition such as corrodibility.
Summary of the invention
The object of the invention is to provide a kind of wide adaptation double-unit system self-lubricating bearing material and preparation method thereof, and the method combines the double mechanism adding solid lubricant and in-situ oxidation reaction, pulverous ZrB
2as body material and provide reaction in－situ self-lubricating mechanism, ZrO
2for toughness reinforcing phase, CaF
2for additive formula self-lubricating batching, prepare applicable self-oiling bearing, and the self-lubricating bearing material that thermal adaptation scope is wider.
A kind of wide adaptation double-unit system self-lubricating bearing material, the volume percent of each raw material of this material is: ZrB
257.0 ~ 70.0%, ZrO
212.0 ~ 37.0%, CaF
26.0%.ZrB
2adopt nano powder, granularity is 40 ~ 50nm; ZrO
2adopt nano powder, granularity is 10 ~ 20nm; CaF
2adopt nano powder, granularity is 150 ~ 155nm.The volume percent of described each raw material is preferably: ZrB
260.0%, ZrO
234.0%, CaF
26.0%.
A kind of wide adaptation double-unit system self-lubricating bearing material, comprises the following steps:
Step one, raw-material pre-treatment
Described ZrB
2nano powder, ZrO
2nano powder and CaF
2nano powder may be mixed with impurity in preparation and wrapping process, and in order to improve its purity, the hydrofluoric acid aqueous solution of employing cleans.Because the granularity of nanopowder is less, activity is comparatively large, and be the corrosion avoiding powder to be subject to hydrofluoric acid, the concentration of hydrofluoric acid should be suitable.Purging method is: respectively by ZrB
2nano powder, ZrO
2nano powder and CaF
2nano powder is placed in the hydrofluoric acid aqueous solution that concentration is 1.8wt%, then 80 ~ 100Hz ultrasonic wave, 100 ~ 120r/min stir process, 90 ~ 100min, leave standstill 60 ~ 90min, pour out upper solution and floating impurity etc., gained throw out adds deionized water and washs, and leaves standstill 60 ~ 90min and again pours out upper solution, again add deionized water and wash, be greater than till 6.5 until upper solution pH value, obtain ZrB after pickling respectively
2nano powder, ZrO
2nano powder and CaF
2nano powder; By ZrB after gained pickling
2nano powder, ZrO
2nano powder and CaF
2nano powder adds absolute ethanol washing once respectively, and then vacuum-drying is 50% to the content mass percent of water, again adds absolute ethanol washing once, then vacuumizes and preserve respectively, obtains ZrB after pre-treatment
2nano powder, ZrO
2nano powder and CaF
2nano powder, for subsequent use;
Step 2, batching, stirring, dispersion and first time ball milling
According to ZrB
2volume percent be 57.0 ~ 70.0%, ZrO
2volume percent be 12.0 ~ 37.0% get pretreated ZrB respectively
2nano powder and ZrO
2nano powder, pours into and ZrB is housed
2nano powder and ZrO
2in the container of the deionized water that nano powder volume of mixture is 2 ~ 4 times, obtain mixture A; This container is combined with temperature sensor, can the temperature of liquid in measuring vessel at any time; Container is placed in ultrasonic generator, 110 ~ 120Hz ultrasonication, 100 ~ 150r/min is carried out to it simultaneously and stir; In ultrasonic agitation process, the temperature of mixture A is increased to 110 DEG C fast, and remains unchanged.After ultrasonic agitation 30 ~ 40min, be 1:90 taking polyethylene glycol according to the mass ratio of polyoxyethylene glycol and mixture A, join in mixture A, continue ultrasonic agitation 10 ~ 20min, obtain mixture B; Gained mixture B is put into ball grinder, take dehydrated alcohol as medium, ball milling 180 ~ 220h, and under 140 ~ 160 DEG C of conditions, vacuum-drying 22 ~ 26h, sieves, and obtains refinement powder, for subsequent use;
Step 3, second time ball milling
According to the volume percent of above-mentioned steps two gained refinement powder be 94%, the CaF that obtains of step one pre-treatment
2the volume percent of nano powder is 6%, gets the CaF that step 2 gained refinement powder and step one pre-treatment obtain
2nano powder, pours the CaF that step 2 gained refinement powder and step one pre-treatment obtain into
2in the container of the deionized water that nano powder cumulative volume is 6 ~ 8 times, obtain mixture C; Described container is combined with temperature sensor, can the temperature of liquid in measuring vessel at any time; The container that mixture C is housed is placed in ultrasonic generator, 80 ~ 100Hz ultrasonic disperse, 100 ~ 150r/min is carried out to it simultaneously and stir; In ultrasonic agitation process, mixture temperature is increased to 100 DEG C fast, maintain this temperature, continue ultrasonic agitation 30 ~ 40min, be that 1:95 adds polyoxyethylene glycol according to the mass ratio of polyoxyethylene glycol and mixture, then continue ultrasonic agitation dispersion 10 ~ 20min, after ultrasonic agitation dispersion terminates, obtain mixture D; Gained mixture D is put into ball grinder, take dehydrated alcohol as medium, ball milling 180 ~ 220h, and under 140 ~ 160 DEG C of conditions, vacuum-drying 22 ~ 26h, sieves, and obtains secondary ball milling refinement powder, for subsequent use;
Step 4: discharge plasma sintering
Step 3 gained secondary ball milling refinement powder is loaded graphite jig, be placed in vacuum environment, then uniform pressurization carries out discharge plasma sintering, during sintering, rise to the process of 1700 DEG C from room temperature, environmental stress even add to 45MPa, afterwards temperature be 1750 DEG C, insulation 10 ~ 25 min under pressure 45MPa condition, then power-off naturally cools to room temperature, namely obtains wide adaptation double-unit system self-lubricating bearing material.
Step 2 and the ball grinder described in step 3 are agate jar;
Described in step 2 and step 3, the method for ball milling is wet type planetary ball mill.
Beneficial effect is:
1, the preparation method of the present invention's wide adaptation double-unit system self-lubricating bearing material, adopts pulverous ZrB
2as body material and provide reaction in－situ self-lubricating mechanism, ZrO
2for toughness reinforcing phase, CaF
2for additive formula self-lubricating batching, and the volume percent controlling each component is: ZrB
260.0 ~ 80.0%, ZrO
215.0 ~ 35.0%, CaF
25.0%, introduce the ZrO of 15.0 ~ 35.0%
2mainly can improve intensity and the toughness of matrix material, ZrB
2the ZrO that also can generate after oxidation
2, make matrix phase ZrB
2with newly-generated ZrO
2, wild phase ZrO
2mutually intert, wrap up, form good skeleton structure, good transformation toughening effect can be formed; Introduce the CaF of 5.0%
2, mainly utilizing this high-temperature lubricating material to provide good self-lubricating when rubbing, utilizing ZrB simultaneously
2/ ZrO
2the support frame effect that ceramic matrix plays, and rely on three ball grinding techniques, by CaF
2solid lubricant is embedded in continuous print ceramic skeleton, can separate out, play the effect of self-lubricating and antifriction when slow cutting or friction.
2, the invention provides the preparation method of wide adaptation double-unit system self-lubricating bearing material, by ZrB
2zrO is added in matrix
2powder and CaF
2powder, and control respective volume fraction, adopt vacuum environment, discharge plasma sintering (SPS) technique of uniform pressurization, this sintering process effectively can reduce the sintering temperature compared with hard-to-sinter boride matrix material, thus obtains the higher material of density; The wide adaptation double-unit system self-lubricating bearing material prepared under these processing condition, be suitable for high/low temperature, have granularity tiny and be evenly distributed, high rigidity, high-flexural strength, high-fracture toughness, the feature such as good high/low temperature stability, be suitable for making higher bearing required to high temperature and wear resistance.
Accompanying drawing explanation
Fig. 1 is the volume percent of each component in raw material: ZrB
255.0%, ZrO
240.0%, CaF
25.0%, constant according in the preparation method of the present invention's wide adaptation double-unit system self-lubricating bearing material of other conditions, prepared material picture after frictional wear under 700 ° of C;
Fig. 2 is wide adaptation double-unit system self-lubricating bearing material picture after frictional wear under 700 ° of C prepared by embodiment two;
Fig. 3 is the volume percent of each component in raw material: ZrB
285.0%, ZrO
210.0%, CaF
25.0%, other conditions are according to the present invention's wide adaptation double-unit system self-lubricating bearing material picture after frictional wear under 700 ° of C;
Fig. 4 is friction temperature and frictional coefficient graph of a relation in high temperature friction and wear experiment;
Fig. 5 is the wide adaptation double-unit system self-lubricating bearing material self lubrication mechanism in friction process-friction initial stage schematic diagram;
Fig. 6 is the self lubrication mechanism-ZrB of wide adaptation double-unit system self-lubricating bearing material in friction process
2, CaF
2particle separates out schematic diagram gradually;
Fig. 7 is the self lubrication mechanism-B of wide adaptation double-unit system self-lubricating bearing material in friction process
2o
3, ZrO
2, CaF
2lubricant film drags at friction surface and covers schematic diagram;
Fig. 8 is the formation schematic diagram of the self lubrication mechanism-self-lubricating film of wide adaptation double-unit system self-lubricating bearing material in friction process;
Fig. 9 is that wide adaptation double-unit system self-lubricating bearing material is oxidized the remaining bending strength figure after 2 hours under 700oC in air;
Figure 10 is remaining fracture toughness property figure after wide adaptation double-unit system self-lubricating bearing material is oxidized 2 hours in air under 700oC.
Embodiment
A kind of wide adaptation double-unit system self-lubricating bearing material, the volume percent of each raw material of this material is: ZrB
257.0 ~ 70.0%, ZrO
212.0 ~ 37.0%, CaF
26.0%.ZrB
2adopt nano powder, granularity is 40 ~ 50nm; ZrO
2adopt nano powder, granularity is 10 ~ 20nm; CaF
2adopt nano powder, granularity is 150 ~ 155nm.The volume percent of described each raw material is preferably: ZrB
260.0%, ZrO
234.0%, CaF
26.0%.
A kind of wide adaptation double-unit system self-lubricating bearing material, comprises the following steps:
Step one, raw-material pre-treatment
Described ZrB
2nano powder, ZrO
2nano powder and CaF
2nano powder may be mixed with impurity in preparation and wrapping process, and in order to improve its purity, the hydrofluoric acid aqueous solution of employing cleans.Because the granularity of nanopowder is less, activity is comparatively large, and be the corrosion avoiding powder to be subject to hydrofluoric acid, the concentration of hydrofluoric acid should be suitable.Purging method is: respectively by ZrB
2nano powder, ZrO
2nano powder and CaF
2nano powder is placed in the hydrofluoric acid aqueous solution that concentration is 1.8wt%, then 80 ~ 100Hz ultrasonic wave, 100 ~ 120r/min stir process, 90 ~ 100min, leave standstill 60 ~ 90min, pour out upper solution and floating impurity etc., gained throw out adds deionized water and washs, and leaves standstill 60 ~ 90min and again pours out upper solution, again add deionized water and wash, be greater than till 6.5 until upper solution pH value, obtain ZrB after pickling respectively
2nano powder, ZrO
2nano powder and CaF
2nano powder; By ZrB after gained pickling
2nano powder, ZrO
2nano powder and CaF
2nano powder adds absolute ethanol washing once respectively, and then vacuum-drying is 50% to the content mass percent of water, again adds absolute ethanol washing once, then vacuumizes and preserve respectively, obtains ZrB after pre-treatment
2nano powder, ZrO
2nano powder and CaF
2nano powder, for subsequent use;
Step 2, batching, stirring, dispersion and first time ball milling
According to ZrB
2volume percent be 57.0 ~ 70.0%, ZrO
2volume percent be 12.0 ~ 37.0% get pretreated ZrB respectively
2nano powder and ZrO
2nano powder, pours into and ZrB is housed
2nano powder and ZrO
2in the container of the deionized water that nano powder volume of mixture is 2 ~ 4 times, obtain mixture A; This container is combined with temperature sensor, can the temperature of liquid in measuring vessel at any time; Container is placed in ultrasonic generator, 110 ~ 120Hz ultrasonication, 100 ~ 150r/min is carried out to it simultaneously and stir; In ultrasonic agitation process, the temperature of mixture A is increased to 110 DEG C fast, and remains unchanged.After ultrasonic agitation 30 ~ 40min, be 1:90 taking polyethylene glycol according to the mass ratio of polyoxyethylene glycol and mixture A, join in mixture A, continue ultrasonic agitation 10 ~ 20min, obtain mixture B; Gained mixture B is put into ball grinder, take dehydrated alcohol as medium, ball milling 180 ~ 220h, and under 140 ~ 160 DEG C of conditions, vacuum-drying 22 ~ 26h, sieves, and obtains refinement powder, for subsequent use;
Step 3, second time ball milling
According to the volume percent of above-mentioned steps two gained refinement powder be 94%, the CaF that obtains of step one pre-treatment
2the volume percent of nano powder is 6%, gets the CaF that step 2 gained refinement powder and step one pre-treatment obtain
2nano powder, pours the CaF that step 2 gained refinement powder and step one pre-treatment obtain into
2in the container of the deionized water that nano powder cumulative volume is 6 ~ 8 times, obtain mixture C; Described container is combined with temperature sensor, can the temperature of liquid in measuring vessel at any time; The container that mixture C is housed is placed in ultrasonic generator, 80 ~ 100Hz ultrasonic disperse, 100 ~ 150r/min is carried out to it simultaneously and stir; In ultrasonic agitation process, mixture temperature is increased to 100 DEG C fast, maintain this temperature, continue ultrasonic agitation 30 ~ 40min, be that 1:95 adds polyoxyethylene glycol according to the mass ratio of polyoxyethylene glycol and mixture, then continue ultrasonic agitation dispersion 10 ~ 20min, after ultrasonic agitation dispersion terminates, obtain mixture D; Gained mixture D is put into ball grinder, take dehydrated alcohol as medium, ball milling 180 ~ 220h, and under 140 ~ 160 DEG C of conditions, vacuum-drying 22 ~ 26h, sieves, and obtains secondary ball milling refinement powder, for subsequent use;
Step 4: discharge plasma sintering
Step 3 gained secondary ball milling refinement powder is loaded graphite jig, be placed in vacuum environment, then uniform pressurization carries out discharge plasma sintering, during sintering, rise to the process of 1700 DEG C from room temperature, environmental stress even add to 45MPa, afterwards temperature be 1750 DEG C, insulation 10 ~ 25 min under pressure 45MPa condition, then power-off naturally cools to room temperature, namely obtains wide adaptation double-unit system self-lubricating bearing material.
Step 2 and the ball grinder described in step 3 are agate jar;
Described in step 2 and step 3, the method for ball milling is wet type planetary ball mill.
embodiment 1
A kind of wide adaptation double-unit system self-lubricating bearing material, the volume percent of each raw material of this material is: ZrB
257.0%, ZrO
237.0%, CaF
26.0%.ZrB
2adopt nano powder, granularity is 40nm; ZrO
2adopt nano powder, granularity is 10nm; CaF
2adopt nano powder, granularity is 150nm.
A kind of wide adaptation double-unit system self-lubricating bearing material, comprises the following steps:
Step one, raw-material pre-treatment
Described ZrB
2nano powder, ZrO
2nano powder and CaF
2nano powder may be mixed with impurity in preparation and wrapping process, and in order to improve its purity, the hydrofluoric acid aqueous solution of employing cleans.Because the granularity of nanopowder is less, activity is comparatively large, and be the corrosion avoiding powder to be subject to hydrofluoric acid, the concentration of hydrofluoric acid should be suitable.Purging method is: respectively by ZrB
2nano powder, ZrO
2nano powder and CaF
2nano powder is placed in the hydrofluoric acid aqueous solution that concentration is 1.8wt%, then 80Hz ultrasonic wave, 100r/min stir process 90min, leave standstill 60min, pour out upper solution and floating impurity etc., gained throw out adds deionized water and washs, and standing 60min pours out upper solution again, again adds deionized water and washs, be greater than till 6.5 until upper solution pH value, obtain ZrB after pickling respectively
2nano powder, ZrO
2nano powder and CaF
2nano powder; By ZrB after gained pickling
2nano powder, ZrO
2nano powder and CaF
2nano powder adds absolute ethanol washing once respectively, and then vacuum-drying is 50% to the content mass percent of water, again adds absolute ethanol washing once, then vacuumizes and preserve respectively, obtains ZrB after pre-treatment
2nano powder, ZrO
2nano powder and CaF
2nano powder, for subsequent use;
Step 2, batching, stirring, dispersion and first time ball milling
According to ZrB
2volume percent be 57.0%, ZrO
2volume percent be 37.0% get pretreated ZrB respectively
2nano powder and ZrO
2nano powder, pours into and ZrB is housed
2nano powder and ZrO
2in the container of the deionized water that nano powder volume of mixture is 2 times, obtain mixture A; This container is combined with temperature sensor, can the temperature of liquid in measuring vessel at any time; Container is placed in ultrasonic generator, 110 ~ 120Hz ultrasonication, 100 ~ 150r/min is carried out to it simultaneously and stir; In ultrasonic agitation process, the temperature of mixture A is increased to 110 DEG C fast, and remains unchanged.After ultrasonic agitation 30 ~ 40min, be 1:90 taking polyethylene glycol according to the mass ratio of polyoxyethylene glycol and mixture A, join in mixture A, continue ultrasonic agitation 10 ~ 20min, obtain mixture B; Gained mixture B is put into ball grinder, take dehydrated alcohol as medium, ball milling 180 ~ 220h, and under 140 ~ 160 DEG C of conditions, vacuum-drying 22 ~ 26h, sieves, and obtains refinement powder, for subsequent use;
Step 3, second time ball milling
According to the volume percent of above-mentioned steps two gained refinement powder be 94%, the CaF that obtains of step one pre-treatment
2the volume percent of nano powder is 6%, gets the CaF that step 2 gained refinement powder and step one pre-treatment obtain
2nano powder, pours the CaF that step 2 gained refinement powder and step one pre-treatment obtain into
2in the container of the deionized water that nano powder cumulative volume is 6 ~ 8 times, obtain mixture C; Described container is combined with temperature sensor, can the temperature of liquid in measuring vessel at any time; The container that mixture C is housed is placed in ultrasonic generator, 80 ~ 100Hz ultrasonic disperse, 100r/min stirring is carried out to it simultaneously; In ultrasonic agitation process, mixture temperature is increased to 100 DEG C fast, maintain this temperature, continue ultrasonic agitation 30 ~ 40min, be that 1:95 adds polyoxyethylene glycol according to the mass ratio of polyoxyethylene glycol and mixture, then continue ultrasonic agitation dispersion 10min, after ultrasonic agitation dispersion terminates, obtain mixture D; Gained mixture D is put into agate jar, take dehydrated alcohol as medium, wet type planetary ball mill 180h, and under 140 DEG C of conditions, vacuum-drying 22h, sieves, and obtains secondary ball milling refinement powder, for subsequent use;
Step 4: discharge plasma sintering
Step 3 gained secondary ball milling refinement powder is loaded graphite jig, be placed in vacuum environment, then uniform pressurization carries out discharge plasma sintering, during sintering, rise to the process of 1700 DEG C from room temperature, environmental stress even add to 45MPa, be 1750 DEG C in temperature, be incubated 10 min under pressure 45MPa condition afterwards, then power-off naturally cools to room temperature, namely obtains wide adaptation double-unit system self-lubricating bearing material.
embodiment 2
A kind of wide adaptation double-unit system self-lubricating bearing material, the volume percent of each raw material of this material is: ZrB
260.0%, ZrO
234.0%, CaF
26.0%.ZrB
2adopt nano powder, granularity is 45nm; ZrO
2adopt nano powder, granularity is 15nm; CaF
2adopt nano powder, granularity is 152nm.
A kind of wide adaptation double-unit system self-lubricating bearing material, comprises the following steps:
Step one, raw-material pre-treatment
Described ZrB
2nano powder, ZrO
2nano powder and CaF
2nano powder may be mixed with impurity in preparation and wrapping process, and in order to improve its purity, the hydrofluoric acid aqueous solution of employing cleans.Because the granularity of nanopowder is less, activity is comparatively large, and be the corrosion avoiding powder to be subject to hydrofluoric acid, the concentration of hydrofluoric acid should be suitable.Purging method is: respectively by ZrB
2nano powder, ZrO
2nano powder and CaF
2nano powder is placed in the hydrofluoric acid aqueous solution that concentration is 1.8wt%, then 90Hz ultrasonic wave, 110r/min stir process 95min, leave standstill 80min, pour out upper solution and floating impurity etc., gained throw out adds deionized water and washs, and standing 80min pours out upper solution again, again adds deionized water and washs, be greater than till 6.5 until upper solution pH value, obtain ZrB after pickling respectively
2nano powder, ZrO
2nano powder and CaF
2nano powder; By ZrB after gained pickling
2nano powder, ZrO
2nano powder and CaF
2nano powder adds absolute ethanol washing once respectively, and then vacuum-drying is 50% to the content mass percent of water, again adds absolute ethanol washing once, then vacuumizes and preserve respectively, obtains ZrB after pre-treatment
2nano powder, ZrO
2nano powder and CaF
2nano powder, for subsequent use;
Step 2, batching, stirring, dispersion and first time ball milling
According to ZrB
2volume percent be 60.0%, ZrO
2volume percent be 34.0% get pretreated ZrB respectively
2nano powder and ZrO
2nano powder, pours into and ZrB is housed
2nano powder and ZrO
2in the container of the deionized water that nano powder volume of mixture is 3 times, obtain mixture A; This container is combined with temperature sensor, can the temperature of liquid in measuring vessel at any time; Container is placed in ultrasonic generator, 110Hz ultrasonication, 100r/min stirring is carried out to it simultaneously; In ultrasonic agitation process, the temperature of mixture A is increased to 110 DEG C fast, and remains unchanged.After ultrasonic agitation 30min, be 1:90 taking polyethylene glycol according to the mass ratio of polyoxyethylene glycol and mixture A, join in mixture A, continue ultrasonic agitation 10min, obtain mixture B; Gained mixture B is put into ball grinder, take dehydrated alcohol as medium, ball milling 200h, and under 140 DEG C of conditions, vacuum-drying 22h, sieves, and obtains refinement powder, for subsequent use;
Step 3, second time ball milling
According to the volume percent of above-mentioned steps two gained refinement powder be 94%, the CaF that obtains of step one pre-treatment
2the volume percent of nano powder is 6%, gets the CaF that step 2 gained refinement powder and step one pre-treatment obtain
2nano powder, pours the CaF that step 2 gained refinement powder and step one pre-treatment obtain into
2in the container of the deionized water that nano powder cumulative volume is 7 times, obtain mixture C; Described container is provided with temperature sensor, can the temperature of liquid in measuring vessel at any time; The container that mixture C is housed is placed in ultrasonic generator, 90Hz ultrasonic disperse, 120r/min stirring is carried out to it simultaneously; In ultrasonic agitation process, mixture temperature is increased to 100 DEG C fast, maintains this temperature, continuing ultrasonic agitation 35min, is that 1:95 adds polyoxyethylene glycol according to the mass ratio of polyoxyethylene glycol and mixture, then continues ultrasonic agitation dispersion 15min, after ultrasonic agitation dispersion terminates, obtain mixture D; Gained mixture D is put into agate jar, take dehydrated alcohol as medium, wet type planetary ball mill 200h, and under 150 DEG C of conditions, vacuum-drying 24h, sieves, and obtains secondary ball milling refinement powder, for subsequent use;
Step 4: discharge plasma sintering
Step 3 gained secondary ball milling refinement powder is loaded graphite jig, be placed in vacuum environment, then uniform pressurization carries out discharge plasma sintering, during sintering, rise to the process of 1700 DEG C from room temperature, environmental stress even add to 45MPa, be 1750 DEG C in temperature, be incubated 20min under pressure 45MPa condition afterwards, then power-off naturally cools to room temperature, namely obtains wide adaptation double-unit system self-lubricating bearing material.
Figure 2 shows that wide adaptation double-unit system self-lubricating bearing material prepared by embodiment two picture after frictional wear under 700 ° of C.Be Al to the material that rubs
2o
3.Comparison diagram 1, the wide adaptation double-unit system self-lubricating bearing material prepared from form embodiment two has good self-lubricating performance after to mill, the distribution of self-lubricating film is comparatively even, does not occur the phenomenon of surface particles severe detachment, the better performances of material monolithic.
embodiment 3
A kind of wide adaptation double-unit system self-lubricating bearing material, the volume percent of each raw material of this material is: ZrB
270.0%, ZrO
224.0%, CaF
26.0%.ZrB
2adopt nano powder, granularity is 50nm; ZrO
2adopt nano powder, granularity is 20nm; CaF
2adopt nano powder, granularity is 155nm.
A kind of wide adaptation double-unit system self-lubricating bearing material, comprises the following steps:
Step one, raw-material pre-treatment
Described ZrB
2nano powder, ZrO
2nano powder and CaF
2nano powder may be mixed with impurity in preparation and wrapping process, and in order to improve its purity, the hydrofluoric acid aqueous solution of employing cleans.Because the granularity of nanopowder is less, activity is comparatively large, and be the corrosion avoiding powder to be subject to hydrofluoric acid, the concentration of hydrofluoric acid should be suitable.Purging method is: respectively by ZrB
2nano powder, ZrO
2nano powder and CaF
2nano powder is placed in the hydrofluoric acid aqueous solution that concentration is 1.8wt%, then 100Hz ultrasonic wave, 120r/min stir process 100min, leave standstill 60 ~ 90min, pour out upper solution and floating impurity etc., gained throw out adds deionized water and washs, and standing 90min pours out upper solution again, again adds deionized water and washs, be greater than till 6.5 until upper solution pH value, obtain ZrB after pickling respectively
2nano powder, ZrO
2nano powder and CaF
2nano powder; By ZrB after gained pickling
2nano powder, ZrO
2nano powder and CaF
2nano powder adds absolute ethanol washing once respectively, and then vacuum-drying is 50% to the content mass percent of water, again adds absolute ethanol washing once, then vacuumizes and preserve respectively, obtains ZrB after pre-treatment
2nano powder, ZrO
2nano powder and CaF
2nano powder, for subsequent use;
Step 2, batching, stirring, dispersion and first time ball milling
According to ZrB
2volume percent be 70.0%, ZrO
2volume percent be 37.0% get pretreated ZrB respectively
2nano powder and ZrO
2nano powder, pours into and ZrB is housed
2nano powder and ZrO
2in the container of the deionized water that nano powder volume of mixture is 2 ~ 4 times, obtain mixture A; This container is combined with temperature sensor, can the temperature of liquid in measuring vessel at any time; Container is placed in ultrasonic generator, 110 ~ 120Hz ultrasonication, 150r/min stirring is carried out to it simultaneously; In ultrasonic agitation process, the temperature of mixture A is increased to 110 DEG C fast, and remains unchanged.After ultrasonic agitation 40min, be 1:90 taking polyethylene glycol according to the mass ratio of polyoxyethylene glycol and mixture A, join in mixture A, continue ultrasonic agitation 20min, obtain mixture B; Gained mixture B is put into ball grinder, take dehydrated alcohol as medium, ball milling 220h, and under 160 DEG C of conditions, vacuum-drying 26h, sieves, and obtains refinement powder, for subsequent use;
Step 3, second time ball milling
According to the volume percent of above-mentioned steps two gained refinement powder be 94%, the CaF that obtains of step one pre-treatment
2the volume percent of nano powder is 6%, gets the CaF that step 2 gained refinement powder and step one pre-treatment obtain
2nano powder, pours the CaF that step 2 gained refinement powder and step one pre-treatment obtain into
2in the container of the deionized water that nano powder cumulative volume is 8 times, obtain mixture C; Described container is combined with temperature sensor, can the temperature of liquid in measuring vessel at any time; The container that mixture C is housed is placed in ultrasonic generator, 100Hz ultrasonic disperse, 150r/min stirring is carried out to it simultaneously; In ultrasonic agitation process, mixture temperature is increased to 100 DEG C fast, maintains this temperature, continuing ultrasonic agitation 40min, is that 1:95 adds polyoxyethylene glycol according to the mass ratio of polyoxyethylene glycol and mixture, then continues ultrasonic agitation dispersion 20min, after ultrasonic agitation dispersion terminates, obtain mixture D; Gained mixture D is put into agate jar, take dehydrated alcohol as medium, wet type planetary ball mill 220h, and under 160 DEG C of conditions, vacuum-drying 26h, sieves, and obtains secondary ball milling refinement powder, for subsequent use;
Step 4: discharge plasma sintering
Step 3 gained secondary ball milling refinement powder is loaded graphite jig, be placed in vacuum environment, then uniform pressurization carries out discharge plasma sintering, during sintering, rise to the process of 1700 DEG C from room temperature, environmental stress even add to 45MPa, afterwards temperature be 1750 DEG C, insulation 10 ~ 25 min under pressure 45MPa condition, then power-off naturally cools to room temperature, namely obtains wide adaptation double-unit system self-lubricating bearing material.
the self lubrication mechanism of the present invention's wide adaptation double-unit system self-lubricating bearing material in friction process
As shown in Fig. 5 to Fig. 8, be the self lubrication mechanism schematic diagram of wide adaptation double-unit system self-lubricating bearing material in friction process, Fig. 5 represents the friction initial stage, and Fig. 6 represents ZrB
2, CaF
2particle is separated out gradually, and Fig. 7 represents B
2o
3, CaF
2, ZrO
2lubricant drags at friction surface and covers, and Fig. 8 represents the formation of self-lubricating film.As shown in Figure 5, when self-lubricating material carries out cutting or rubbing, between friction pair, a large amount of heat of friction can be produced, be in the effect that self-lubricating material top layer is subject to heat of friction and stress, TiB
2, ZrB
2particle is separated out gradually; As shown in Figure 6, under the effect of High Temperature High Pressure and oxygen, easily there is friction chemical reaction, generate the ZrB with lubrication at material surface
2, CaF
2, ZrO
2lubricant film; As shown in Figure 7, after friction, due to the hardness of solid lubricant and shearing resistance lower, so separate out surperficial solid lubricant under rubbing effect, be easy to be dragged overlay on friction surface, when a large amount of solid lubricant particle dragged cover time, just define lubricant film at friction surface; As shown in Figure 8, be no matter form complete lubricant film between surface of friction, or forming section lubricant 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 99.5004323A8ure, zirconium white, Calcium Fluoride (Fluorspan), the double mechanism self-lubricating of the solid lubricant under high temperature friction effect and in-situ oxidation reaction, the reaction film with lubrication is generated at material surface, thus realizing self-lubricating, correlation technique can be prepared one and not only be applicable to high speed cutting but also also unrestricted to wide adaptation double-unit system self-lubricating bearing material at low temperature.
related experiment
1, the present invention's wide adaptation double-unit system self-lubricating bearing material high temperature friction and wear experiment:
Friction-wear test is carried out in UMT-2 Multifunctional friction experimental machine (U.S., CETR company).The working range of this frictional testing machines sensor is at 0 ~ 200N, and precision can reach 10mN; Level and vertical displacement precision are 0.1mm/s; The speed of mainshaft is at 0 ~ 5000rev/min, and precision can reach 0.1 rev/min; The working range of heating chamber is at 0 ~ 1000 DEG C, and precision is 0.1 DEG C.Infrared temperature detection system precision is 0.5 DEG C.The secondary form of joining of friction selects ball-dish friction-type.To the material that rubs: Al
2o
3.Four groups of materials are selected in experiment respectively, and one group is pure ZrB
2,two groups to be the volume percent of raw material be: ZrB
255.0%, ZrO
240.0%, CaF
25.0%, preparation method is identical with the present invention for other compositions; Three groups is the present invention's wide adaptation double-unit system self-lubricating bearing material; Four groups to be the volume percent of raw material be: ZrB
265.0%, ZrO
230.0%, CaF
25.0%, preparation method is identical with the present invention for other compositions; Its result as shown in Figure 4 high temperature friction and wear experiment in frictional coefficient and friction temperature graph of a relation.As can be seen from the figure, general ZrB
2there is reaction in－situ at 500 ~ 700 DEG C, form reaction in－situ self-lubricating.But 500 DEG C time, pure ZrB
2with Al
2o
3to when rubbing, owing to not there is self-lubricating, frictional coefficient reaches 0.65, the present invention's wide adaptation double-unit system self-lubricating bearing material, time below 500 DEG C, and the solid lubricant CaF of interpolation
2lubricant film can be generated, therefore frictional coefficient is starkly lower than pure ZrB
2.And the present invention's wide adaptation double-unit system self-lubricating bearing material, higher than after 700 DEG C, all can there is reaction in－situ in temperature.As can be seen from the figure material of the present invention is in temperature higher than 700 DEG C, and all can show good self-lubricating property lower than when 500 DEG C, is good cutter material;
2, the present invention's wide adaptation double-unit system self-lubricating bearing material oxidation experiment in air under 700oC:
Material in this experiment, other compositions and preparation method are all identical with of the present invention, ZrO
2volume percent content different; Experimental result is as shown in Fig. 9 and Figure 10, and this figure is respectively different ZrO
2the material of content is oxidized the remaining bending strength figure after 2 hours and remaining fracture toughness property figure under 700oC in air; As can be seen from the figure, ZrB is worked as
2for volume percent content be 30% time oxidation after residual mechanical properties best, than (ZrB
295vol.%+ CaF
25vol.%) the remaining bending strength of stupalith improves 88.3%, and remaining fracture toughness property improves 96.9%.Experiment proves, the present invention's wide adaptation double-unit system self-lubricating bearing material has stronger bending strength and remaining fracture toughness property.
3, test when preparation method's Raw component proportions of the present invention's wide adaptation double-unit system self-lubricating bearing material changes:
(1), when the volume percent of component each in raw material is: ZrB
255.0%, ZrO
240.0%, CaF
25.0%, constant according in the preparation method of the present invention's wide adaptation double-unit system self-lubricating bearing material of other conditions, prepared material, carries out frictional wear experiment under 700 ° of C, is Al to the material that rubs
2o
3; Fig. 1 is experimental result; According to EDX figure and the known Fig. 1 of X-ray diffraction in black region be ZrO
2, canescence region is ZrB
2, white reflection region is CaF
2.As can be seen from Figure 1, between the crystal grain after high temperature friction and wear experiment, the combination degree at interface weakens to some extent, and there is the phenomenon of particle detachment on surface, does not show good double-unit system self-lubricating effect from form.Main because work as ZrO
2content more than 35% time, ZrO
2the feature that the hardness of material own is lower just shows, although ZrO
2there is the effect of transformation toughening, but the bulk strength of material is still under some influence after high temperature friction and wear.
(2), when the volume percent of component each in raw material is: ZrB
285.0%, ZrO
210.0%, CaF
25.0%, constant according in the preparation method of the present invention's wide adaptation double-unit system self-lubricating bearing material of other conditions, prepared material, carries out frictional wear experiment under 700 ° of C, is Al to the material that rubs
2o
3; Fig. 3 is experimental result; Comparison diagram 2, prepared material is through comparatively serious to the wearing and tearing dropping situations of material after rubbing, and the density of material is more less better than the wide adaptation double-unit system self-lubricating bearing material prepared by the present invention, does not show good double-unit system self-lubricating effect.Work as ZrB
2content more than 80% time, ZrB
2the more difficult feature of the densification of material own just shows, although a small amount of ZrO
2there is the effect of transformation toughening, but the bulk strength of material is still under some influence after high temperature friction and wear.
Claims (6)
1. a wide adaptation double-unit system self-lubricating bearing material, is characterized in that: the volume percent of each raw material of this material is: ZrB
257.0 ~ 70.0%, ZrO
212.0 ~ 37.0%, CaF
26.0%; ZrB
2adopt nano powder, granularity is 40 ~ 50nm; ZrO
2adopt nano powder, granularity is 10 ~ 20nm; CaF
2adopt nano powder, granularity is 150 ~ 155nm.
2. a kind of wide adaptation double-unit system self-lubricating bearing material as claimed in claim 1, is characterized in that: the volume percent of described each raw material is preferably: ZrB
260.0%, ZrO
234.0%, CaF
26.0%.
3. the preparation method of a kind of wide adaptation double-unit system self-lubricating bearing material as claimed in claim 1 or 2, is characterized in that: comprise the following steps:
Step one, raw-material pre-treatment
Respectively by ZrB
2nano powder, ZrO
2nano powder and CaF
2nano powder is placed in the hydrofluoric acid aqueous solution that concentration is 1.8wt%, then 80 ~ 100Hz ultrasonic wave, 100 ~ 120r/min stir process, 90 ~ 100min, leave standstill 60 ~ 90min, pour out upper solution and floating impurity, gained throw out adds deionized water and washs, and leaves standstill 60 ~ 90min and again pours out upper solution, again add deionized water and wash, be greater than till 6.5 until upper solution pH value, obtain ZrB after pickling respectively
2nano powder, ZrO
2nano powder and CaF
2nano powder; By ZrB after gained pickling
2nano powder, ZrO
2nano powder and CaF
2nano powder adds absolute ethanol washing respectively, obtains ZrB after pre-treatment
2nano powder, ZrO
2nano powder and CaF
2nano powder, for subsequent use;
Step 2, batching, stirring, dispersion and first time ball milling
According to ZrB
2volume percent be 57.0 ~ 70.0%, ZrO
2volume percent be 12.0 ~ 37.0% get pretreated ZrB respectively
2nano powder and ZrO
2nano powder, pours into and ZrB is housed
2nano powder and ZrO
2the deionized water that nano powder volume of mixture is 2 ~ 4 times and be provided with in the container of temperature sensor, obtains mixture A; The container that mixture A is housed is placed in ultrasonic generator, 110 ~ 120Hz ultrasonication, 100 ~ 150r/min is carried out to it simultaneously and stir; In ultrasonic agitation process, the temperature of mixture A is increased to 110 DEG C, maintains this temperature, ultrasonic agitation 30 ~ 40min is 1:90 taking polyethylene glycol according to the mass ratio of polyoxyethylene glycol and mixture A, joins in mixture A, continue ultrasonic agitation 10 ~ 20min, obtain mixture B; Gained mixture B is put into ball grinder, take dehydrated alcohol as medium, ball milling 180 ~ 220h, and under 140 ~ 160 DEG C of conditions, vacuum-drying 22 ~ 26h, sieves, and obtains refinement powder, for subsequent use;
Step 3, second time ball milling
According to the volume percent of above-mentioned steps two gained refinement powder be 94%, the CaF that obtains of step one pre-treatment
2the volume percent of nano powder is 6%, gets the CaF that step 2 gained refinement powder and step one pre-treatment obtain
2nano powder, pours the CaF that step 2 gained refinement powder and step one pre-treatment obtain into
2in the container of the deionized water that nano powder cumulative volume is 6 ~ 8 times, obtain mixture C; Described container is provided with temperature sensor; The container that mixture C is housed is placed in ultrasonic generator, 80 ~ 100Hz ultrasonication, 100 ~ 150r/min is carried out to it simultaneously and stir; In ultrasonic agitation process, mixture temperature is increased to 100 DEG C, maintain this temperature, continue ultrasonic agitation 30 ~ 40min, be that 1:95 adds polyoxyethylene glycol according to the mass ratio of polyoxyethylene glycol and mixture, then continue ultrasonic agitation dispersion 10 ~ 20min, after ultrasonic agitation dispersion terminates, obtain mixture D; Gained mixture D is put into ball grinder, take dehydrated alcohol as medium, ball milling 180 ~ 220h, and under 140 ~ 160 DEG C of conditions, vacuum-drying 22 ~ 26h, sieves, and obtains secondary ball milling refinement powder, for subsequent use;
Step 4: discharge plasma sintering
Step 3 gained secondary ball milling refinement powder is loaded graphite jig, be placed in vacuum environment, then uniform pressurization carries out discharge plasma sintering, during sintering, rise to the process of 1700 DEG C from room temperature, environmental stress even add to 45MPa, afterwards temperature be 1750 DEG C, insulation 10 ~ 25 min under pressure 45MPa condition, then power-off naturally cools to room temperature, namely obtains wide adaptation double-unit system self-lubricating bearing material.
4. the preparation method of wide adaptation double-unit system self-lubricating bearing material as claimed in claim 3, is characterized in that: step 2 and the ball grinder described in step 3 are agate jar.
5. the preparation method of wide adaptation double-unit system self-lubricating bearing material as claimed in claim 3, is characterized in that: described in step 2 and step 3, the method for ball milling is wet type planetary ball mill.
6. the preparation method of wide adaptation double-unit system self-lubricating bearing material as claimed in claim 3, is characterized in that: described by ZrB after gained pickling
2nano powder, ZrO
2nano powder and CaF
2the method that nano powder adopts dehydrated alcohol to carry out washing is: add absolute ethanol washing respectively once, then vacuum-drying is 50% to the content mass percent of water, again adds absolute ethanol washing once, then vacuumizes and preserve respectively, for subsequent use.
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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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| Publication number | Priority date | Publication date | Assignee | Title |
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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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| CN107365917A (en) * | 2017-06-30 | 2017-11-21 | 常州瑞坦商贸有限公司 | A kind of preparation method of wear-resisting type metal-based Self-lubricating Bearing material |
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