CN108555294A - A kind of self-lubricating ceramic material and preparation method thereof - Google Patents

A kind of self-lubricating ceramic material and preparation method thereof Download PDF

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CN108555294A
CN108555294A CN201810412218.6A CN201810412218A CN108555294A CN 108555294 A CN108555294 A CN 108555294A CN 201810412218 A CN201810412218 A CN 201810412218A CN 108555294 A CN108555294 A CN 108555294A
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powder
self
parts
lubricating
molybdenum disulfide
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沈春霞
王文新
蔡静
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Foshan Nine Mo Science And Technology Information Consulting Co Ltd
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Foshan Nine Mo Science And Technology Information Consulting Co Ltd
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Abstract

The present invention relates to a kind of self-lubricating ceramic materials and preparation method thereof, belong to metallurgical technology field.The present invention is by 3D printing technique by alumina powder, molybdenum powder is laid in the cellular structural material that 3D printing is carried out in selective laser sintering and moulding equipment into spacial ordering, recycle class graphene-structured molybdenum disulfide, silver, barium sulfate, the composite powder of eutectic powder composition is as kollag, utilize the synergistic effect of the kollag of itself anti-wear and wear-resistant performance and filling of the orderly honeycomb of space surface, material can be further decreased in room temperature, friction coefficient under medium temperature, and then realize the laminar composite in room temperature to the continuous self-lubricating in 800 DEG C of temperature ranges；The present invention is diffused into surface from coat inside using silver and forms one layer of continuous lubricating film, which can inhibit the oxidation of molybdenum, also be improved the nano hardness of material and elasticity modulus, mechanical property gets a promotion.

Description

A kind of self-lubricating ceramic material and preparation method thereof
Technical field
The present invention relates to a kind of self-lubricating ceramic materials and preparation method thereof, belong to metallurgical technology field.
Background technology
A total of about 1,500,000,000 tons of all kinds of fuel oils that the whole world consumes every year, but effective utilization rate of energy only has 30% or so.According to estimating Meter, friction and wear consume the 30%~40% of the consumed worldwide energy.Lubrication is to improve tribological property most straightforward approach. Traditional system maintenance and lubricating method is regular addition lubricant grease etc., but the maintenance of this method is cumbersome, and lubricating oil is in height The lower performance of temperature declines, and makes equipment that occlusion etc. occur and lubrication failure occurs, be not suitable with the development of science and technology.The development of modern industry, it is right More stringent requirements are proposed for the various antifriction materials used under high temperature operating conditions, to make the lubrication of material under the high temperature conditions Problem is paid more and more attention, such as pyrometallurgy, high temperature chemical machinery, vacuum operating bearing, air cooling engine, electric conductivity slide plate and permitted More careless quarter working conditions, it is stuck with bearing that this can cause bearing retainer to distort, and has seriously affected the mutual operating that part is asked, Larger abrasion is caused, larger loss is brought to enterprise.
Metal-based self-lubricating material is applicable under different careless quarter environment, type and application because of its unique property For range than wide, apparent advantage is apparent in preparation and application etc., such as the relatively low and anti-rotten candle energy of the density of polymer Power is preferable, but its mechanical strength is low, and is easy failing under the conditions of temperature is higher；Ceramic based self-lubricating material it is resistance to Corrosivity and wearability are higher, but the manufacturing cost of material is higher, and the difficulty of processing after preparation is bigger.And metal-based self-lubricating The toughness and plasticity of material are preferable, and easy to process, toughness is preferable, and mechanical property can carry lubricating film, and wearability is preferable, energy It is enough to be used under various special or careless quarter environment.In addition, part metals can also be formed in friction process it is a variety of have lubrication The compound of property, improves the greasy property of material.
It is with the development of modern industry and progressive, it needs to develop the better solid self lubricant material of tribological property, It is the main research of tribological field to rub, wear, lubricating, and solid lubrication is wherein main part.Solid moistens certainly Sliding material is typically to be allowed to kollag between being placed in two friction surfaces by the special process such as being sintered, being electroplated, and is reduced Two load-bearing surfaces are in direct contact, the limitation of development and conventional grease lubrication due to solid lubricant, Yi Jigu Body self-lubricating material causes tribological field pass in some careless applications carved under working condition, the research of solid self lubricant material Note.
In mechanical industry, properties of solid self-lubricant coating technology of preparing, the operational safety of equipment, reliability and using energy source are all Associated with the research of tribology, the development of modern industrial technology makes the friction, abrasion and lubrication problem of equipment by higher Pay attention to, especially in such as high temperature and pressure of the use under special operation condition etc..General lubricating oil, lubricating grease etc. are because under high temperature environment Vulnerable and volatilization, and be difficult under conditions of dust and larger impact strength to play lubricating action, general lubricant grease makes With temperature between 50 DEG C~350 DEG C of ﹣, dry friction makes equipment generate serious abrasion, shortens the service life of equipment, causes wave Take, and be easy to cause safety accident, therefore, the friction, abrasion, the research significance of lubrication problem under hot conditions are great.
Invention content
The technical problems to be solved by the invention：For pyrometallurgy, high temperature chemical machinery, vacuum operating bearing, air-cooled start Machine and many careless quarter working conditions can cause bearing retainer to distort stuck with bearing, seriously affect the phase between part Mutually operating, the problem of causing larger abrasion, provide a kind of self-lubricating ceramic material and preparation method thereof.
In order to solve the above technical problems, the technical solution adopted by the present invention is：
A kind of self-lubricating ceramic material includes ceramic matrix material and composite powder, and the composite powder is by following weight parts original Material composition：7.5~15.0 parts of class graphene-structured molybdenum disulfide, 2.5~5.0 parts of silver, 5~10 parts of barium sulfate, 35~70 parts altogether Crystalline flour.
The ceramic matrix material is that matrix powder is laid in selective laser sintering and moulding equipment 3D printing into space Orderly cellular structural material, print parameters are：0.05~0.10mm of sweep span, 0.05~0.10mm of lift height, scanning 1500~2000mm/min of speed, powder preheating temperature are 1400~1500 DEG C.
Described matrix powder is by alumina powder and molybdenum powder in mass ratio 2：1 mixing and ball milling is made.
The class graphene-structured molybdenum disulfide is that molybdenum disulfide ultrasound stripping in cholic acid sodium water solution is made, described two Molybdenum sulfide, sodium taurocholate, deionized water parts by weight be 20~30 parts of molybdenum disulfide powders, 6~9 parts of sodium taurocholates, 4000~6000 Part deionized water.
The eutectic powder is by 25~30 parts by weight calcirm-fluoride, and 70~75 parts by weight barium fluorides after mixing grind by vacuum-sintering It grinds.
The composite powder dosage is the 1~5% of ceramic matrix material quality.
A kind of preparation method of the self-lubricating ceramic material, the specific steps are：
（1）It takes alumina powder, molybdenum powder to be fitted into planetary ball mill, adds absolute ethyl alcohol wet ball grinding 12~do afterwards for 24 hours It is dry, obtain matrix powder；
（2）Matrix powder is laid in the honeycomb that 3D printing is carried out in selective laser sintering and moulding equipment into spacial ordering Material obtains ceramic matrix material；
（3）It takes molybdenum disulfide powder, sodium taurocholate to be added in deionized water, is centrifuged after ultrasonic disperse, collect precipitation and drying, Obtain class graphene-structured molybdenum disulfide；
（4）Calcirm-fluoride, barium fluoride are taken, is fitted into batch mixer and is uniformly mixed, then is sintered 30~40min at 1100~1200 DEG C, 3~5h is ground after cooling, obtains eutectic powder；
（5）Class graphene-structured molybdenum disulfide, silver, barium sulfate, eutectic powder are taken, is fitted into batch mixer and is uniformly mixed, obtain composite powder End takes composite powder uniformly to rub in ceramic matrix material surface, then is placed in vacuum heating-press sintering machine, is heated up with 20 DEG C/min To 1200~1300 DEG C, 20~30min of hot pressing is kept the temperature at 20~30MPa, is taken out after being cooled to room temperature, obtains self-lubrication ceramic material Material.
Compared with other methods, advantageous effects are the present invention：
（1）The present invention by 3D printing technique by alumina powder, molybdenum powder be laid in selective laser sintering and moulding equipment into Row 3D printing recycles class graphene-structured molybdenum disulfide, silver, barium sulfate, eutectic powder at the cellular structural material of spacial ordering The composite powder of composition as kollag, using the orderly honeycomb of space surface itself anti-wear and wear-resistant performance and fill out The synergistic effect of the kollag filled can further decrease friction coefficient of the material under room temperature, medium temperature, and then realize the layer Shape composite material is in room temperature to the continuous self-lubricating in 800 DEG C of temperature ranges；
（2）The present invention is diffused into surface from coat inside using silver and forms one layer of continuous lubricating film, which can inhibit The oxidation of molybdenum, when temperature is increased to 500 DEG C or more, the abrasion of coating aggravates, and the aerial molybdenum high-temperature oxydation of exposure generates Molybdenum trioxide and silver molybdate the lubricant effect under higher temperature can be provided, sulphur wherein in class graphene-structured molybdenum disulfide member Element has catalytic action for the formation of silver molybdate, and class graphene-structured molybdenum disulfide forms mild method in surface of friction pair Film reduces friction coefficient with this, plays and fills up and repair to friction surface, also makes the nano hardness and elasticity modulus of material It is improved, mechanical property gets a promotion.
Specific implementation mode
2~3kg alumina powders, 1.0~1.5kg molybdenum powders is taken to be fitted into planetary ball mill, add 50~100mL Product is taken out after ball milling, is placed in drying box, 70 with 150~200r/min ball millings 12~for 24 hours by absolute ethyl alcohol Dry 15~20h, obtains matrix powder, matrix powder is laid in selective laser sintering and moulding equipment and carries out 3D at~75 DEG C Printing shaping, control print parameters are as follows：0.05~0.10mm of sweep span, 0.05~0.10mm of lift height, sweep speed 1500~2000mm/min, powder preheating temperature are 1400~1500 DEG C, and matrix powder is printed as to the honeycomb knot of spacial ordering Structure material, obtains ceramic matrix material, and 20~30g molybdenum disulfide powders, 6~9g sodium taurocholates is taken to be added in 4~6L deionized waters, Under 40~50 DEG C of waters bath with thermostatic control, after disperseing 6~8h with 400W ultrasonic echographies, it is transferred in centrifuge, with 3000~4000r/ Min centrifuge 20~30min, collect supernatant, then by supernatant with 10000~12000r/min centrifuge 30~ 40min collects precipitation, precipitation is placed in drying box, is dried to constant weight at 105~110 DEG C, obtains two sulphur of class graphene-structured Change molybdenum, 25~30g calcirm-fluoride, 70~75g barium fluorides is taken to be fitted into batch mixer and be uniformly mixed, then be transferred in vacuum sintering furnace, It is sintered 30~40min at 1100~1200 DEG C, sintered product is taken out after being cooled to room temperature, and is fitted into 3~5h of grinding in grinder, Eutectic powder is obtained, 7.5~15.0g class graphene-structured molybdenum disulfide is taken, 2.5~5.0g is silver-colored, 5~10g barium sulfate, and 35~70g is total Crystalline flour is fitted into batch mixer and is uniformly mixed, obtains composite powder, and composite powder is taken uniformly to rub in ceramic matrix material surface, control Composite powder dosage processed is the 1~5% of ceramic matrix material quality, then is placed in vacuum heating-press sintering machine, is heated up with 20 DEG C/min To 1200~1300 DEG C, 20~30min of hot pressing is kept the temperature at 20~30MPa, is taken out after being cooled to room temperature, obtains self-lubrication ceramic material Material.
It takes 2kg alumina powders, 1.0kg molybdenum powders to be fitted into planetary ball mill, adds 50mL absolute ethyl alcohols, with Product is taken out after ball milling, is placed in drying box by 150r/min ball milling 12h, and dry 15h, obtains matrix powder at 70 DEG C Matrix powder is laid in progress 3D printing molding in selective laser sintering and moulding equipment by end, and control print parameters are as follows：It sweeps Spacing 0.05mm, lift height 0.05mm, sweep speed 1500mm/min are retouched, powder preheating temperature is 1400 DEG C, by matrix powder End is printed as the cellular structural material of spacial ordering, obtains ceramic matrix material, and 20g molybdenum disulfide powders, 6g sodium taurocholates is taken to be added In 4L deionized waters, under 40 DEG C of waters bath with thermostatic control, after disperseing 6h with 400W ultrasonic echographies, it is transferred in centrifuge, with 3000r/ Min centrifuges 20min, collects supernatant, then supernatant is centrifuged 30min with 10000r/min, collects precipitation, will sink Shallow lake is placed in drying box, is dried to constant weight at 105 DEG C, is obtained class graphene-structured molybdenum disulfide, and 25g calcirm-fluoride, 70g fluorinations are taken Barium is fitted into batch mixer and is uniformly mixed, then is transferred in vacuum sintering furnace, is sintered 30min at 1100 DEG C, is taken after being cooled to room temperature Go out sintered product, and be fitted into grinder and grind 3h, obtain eutectic powder, takes 7.5g class graphene-structured molybdenum disulfide, 2.5g silver, 5g Barium sulfate, 35g eutectic powder are fitted into batch mixer and are uniformly mixed, obtain composite powder, composite powder is taken uniformly to rub in ceramic matrix Material surface, control composite powder dosage is the 1% of ceramic matrix material quality, then is placed in vacuum heating-press sintering machine, with 20 DEG C/min is warming up to 1200 DEG C, hot pressing 20min is kept the temperature at 20MPa, is taken out after being cooled to room temperature, is obtained self-lubricating ceramic material.
It takes 2kg alumina powders, 1.2kg molybdenum powders to be fitted into planetary ball mill, adds 80mL absolute ethyl alcohols, with Product is taken out after ball milling, is placed in drying box by 180r/min ball milling 18h, and dry 18h, obtains matrix powder at 72 DEG C Matrix powder is laid in progress 3D printing molding in selective laser sintering and moulding equipment by end, and control print parameters are as follows：It sweeps Spacing 0.08mm, lift height 0.08mm, sweep speed 1800mm/min are retouched, powder preheating temperature is 1450 DEG C, by matrix powder End is printed as the cellular structural material of spacial ordering, obtains ceramic matrix material, and 25g molybdenum disulfide powders, 8g sodium taurocholates is taken to be added In 5L deionized waters, under 45 DEG C of waters bath with thermostatic control, after disperseing 7h with 400W ultrasonic echographies, it is transferred in centrifuge, with 3500r/ Min centrifuges 25min, collects supernatant, then supernatant is centrifuged 35min with 11000r/min, collects precipitation, will sink Shallow lake is placed in drying box, is dried to constant weight at 108 DEG C, is obtained class graphene-structured molybdenum disulfide, and 28g calcirm-fluoride, 72g fluorinations are taken Barium is fitted into batch mixer and is uniformly mixed, then is transferred in vacuum sintering furnace, is sintered 35min at 1150 DEG C, is taken after being cooled to room temperature Go out sintered product, and be fitted into grinder and grind 4h, obtain eutectic powder, takes 10g class graphene-structured molybdenum disulfide, 4g silver, 8g sulphur Sour barium, 55g eutectic powder are fitted into batch mixer and are uniformly mixed, obtain composite powder, composite powder is taken uniformly to rub in ceramic matrix material Expect surface, control composite powder dosage is the 3% of ceramic matrix material quality, then is placed in vacuum heating-press sintering machine, with 20 DEG C/ Min is warming up to 1250 DEG C, and hot pressing 25min is kept the temperature at 25MPa, is taken out after being cooled to room temperature, obtains self-lubricating ceramic material.
It takes 3kg alumina powders, 1.5kg molybdenum powders to be fitted into planetary ball mill, adds 100mL absolute ethyl alcohols, with 200r/min ball millings for 24 hours, take out product after ball milling, are placed in drying box, and dry 20h, obtains matrix powder at 75 DEG C Matrix powder is laid in progress 3D printing molding in selective laser sintering and moulding equipment by end, and control print parameters are as follows：It sweeps Spacing 0.10mm, lift height 0.10mm, sweep speed 2000mm/min are retouched, powder preheating temperature is 1500 DEG C, by matrix powder End is printed as the cellular structural material of spacial ordering, obtains ceramic matrix material, and 30g molybdenum disulfide powders, 9g sodium taurocholates is taken to be added In 6L deionized waters, under 50 DEG C of waters bath with thermostatic control, after disperseing 8h with 400W ultrasonic echographies, it is transferred in centrifuge, with 4000r/ Min centrifuges 30min, collects supernatant, then supernatant is centrifuged 40min with 12000r/min, collects precipitation, will sink Shallow lake is placed in drying box, is dried to constant weight at 110 DEG C, is obtained class graphene-structured molybdenum disulfide, and 30g calcirm-fluoride, 75g fluorinations are taken Barium is fitted into batch mixer and is uniformly mixed, then is transferred in vacuum sintering furnace, is sintered 40min at 1200 DEG C, is taken after being cooled to room temperature Going out sintered product, and be fitted into grinder and grind 5h, obtain eutectic powder, takes 15.0g class graphene-structured molybdenum disulfide, 5.0g is silver-colored, 10g barium sulfate, 70g eutectic powder are fitted into batch mixer and are uniformly mixed, obtain composite powder, composite powder is taken uniformly to rub in ceramics Substrate material surface, control composite powder dosage is the 5% of ceramic matrix material quality, then is placed in vacuum heating-press sintering machine, with 20 DEG C/min is warming up to 1300 DEG C, and hot pressing 30min is kept the temperature at 30MPa, is taken out after being cooled to room temperature, obtains self-lubrication ceramic material Material.
Reference examples：The self-lubricating ceramic material of Dongguan company production.
The self-lubricating ceramic material of example and reference examples is detected, specific detection is as follows：
Determination of Hardness：Using digital display small-load Brinell hardenss tester, by the size of manual measurement impression, then calculate automatically hard Angle value can calculate average value automatically after measuring three times.The setting condition of test is load 62.5Kg, and the ballast time is 30s, pressure Bulb diameter 2.5mm.3~5 points are taken in the different parts of material sample when measurement, are then averaged.The calculating of Brinell hardness Method is calculated generally according to formula.
Compression strength：It is the leading indicator for testing lubriation material, is primarily referred to as applying strength degree when pressure.Composite wood The compression strength of material is tested according to national standard GB/T6569-86, and form is mainly with cylindrical sample in axial compressive force The peak load divided by the obtained stress of original sample cross-sectional area born when under effect.
Frictional behaviour is tested：The friction and wear behavior experiment of material is tested using instrument for XW-3 type high temperature friction and wears Machine.
Specific testing result such as table 1.
1 performance characterization contrast table of table
Detection project Example 1 Example 2 Example 3 Reference examples
Hardness HB 177 171 167 101
Compression strength MPa 573 558 551 470
Average friction coefficient 0.35 0.39 0.41 0.65
As shown in Table 1, the self-lubricating ceramic material hardness that prepared by the present invention is high, and compression strength is good, and average friction coefficient is small, has Good mechanical property and tribological property.

Claims (7)

1. a kind of self-lubricating ceramic material, which is characterized in that including ceramic matrix material and composite powder, the composite powder by Following weight parts raw material forms：7.5~15.0 parts of class graphene-structured molybdenum disulfide, 2.5~5.0 parts of silver, 5~10 parts of sulfuric acid Barium, 35~70 parts of eutectic powder.
2. a kind of self-lubricating ceramic material as described in claim 1, which is characterized in that the ceramic matrix material is matrix powder End is laid in the cellular structural material of 3D printing in selective laser sintering and moulding equipment at spacial ordering, and print parameters are：It sweeps Retouch 0.05~0.10mm of spacing, 0.05~0.10mm of lift height, 1500~2000mm/min of sweep speed, powder preheating temperature It is 1400~1500 DEG C.
3. a kind of self-lubricating ceramic material as claimed in claim 2, which is characterized in that described matrix powder is by alumina powder With molybdenum powder in mass ratio 2：1 mixing and ball milling is made.
4. a kind of self-lubricating ceramic material as described in claim 1, which is characterized in that the class graphene-structured molybdenum disulfide For molybdenum disulfide in cholic acid sodium water solution ultrasound stripping be made, the molybdenum disulfide, sodium taurocholate, deionized water parts by weight be 20~30 parts of molybdenum disulfide powders, 6~9 parts of sodium taurocholates, 4000~6000 parts of deionized waters.
5. a kind of self-lubricating ceramic material as described in claim 1, which is characterized in that the eutectic powder is by 25~30 parts by weight Calcirm-fluoride, vacuum-sintering grinding is made 70~75 parts by weight barium fluorides after mixing.
6. a kind of self-lubricating ceramic material as described in claim 1, which is characterized in that the composite powder dosage is ceramic base The 1~5% of body quality of materials.
7. a kind of preparation method of self-lubricating ceramic material as described in claim 1~6 any one, which is characterized in that tool Body step is：
（1）It takes alumina powder, molybdenum powder to be fitted into planetary ball mill, adds absolute ethyl alcohol wet ball grinding 12~do afterwards for 24 hours It is dry, obtain matrix powder；
（2）Matrix powder is laid in the honeycomb that 3D printing is carried out in selective laser sintering and moulding equipment into spacial ordering Material obtains ceramic matrix material；
（3）It takes molybdenum disulfide powder, sodium taurocholate to be added in deionized water, is centrifuged after ultrasonic disperse, collect precipitation and drying, Obtain class graphene-structured molybdenum disulfide；
（4）Calcirm-fluoride, barium fluoride are taken, is fitted into batch mixer and is uniformly mixed, then is sintered 30~40min at 1100~1200 DEG C, 3~5h is ground after cooling, obtains eutectic powder；
（5）Class graphene-structured molybdenum disulfide, silver, barium sulfate, eutectic powder are taken, is fitted into batch mixer and is uniformly mixed, obtain composite powder End takes composite powder uniformly to rub in ceramic matrix material surface, then is placed in vacuum heating-press sintering machine, is heated up with 20 DEG C/min To 1200~1300 DEG C, 20~30min of hot pressing is kept the temperature at 20~30MPa, is taken out after being cooled to room temperature, obtains self-lubrication ceramic material Material.
CN201810412218.6A 2018-05-03 2018-05-03 A kind of self-lubricating ceramic material and preparation method thereof Pending CN108555294A (en)

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CN110922846A (en) * 2019-12-23 2020-03-27 山东库克斯节能环保科技有限公司 Water pump polymer super-smooth energy-saving ceramic coating material and use method thereof

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AU4375599A (en) * 1998-06-29 2000-01-17 Radiance Composite blade, capable of being used in different technical or industrial fields, in particular in the paper industry and printing
CN106086526A (en) * 2016-07-26 2016-11-09 中国科学院兰州化学物理研究所 A kind of high temperature resistant wide temperature range self-lubricating composite and preparation method thereof
CN106244885A (en) * 2016-07-28 2016-12-21 中国科学院兰州化学物理研究所 A kind of multiple structure aluminium oxide self-lubricating composite ceramic and preparation method thereof
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AU4375599A (en) * 1998-06-29 2000-01-17 Radiance Composite blade, capable of being used in different technical or industrial fields, in particular in the paper industry and printing
CN106086526A (en) * 2016-07-26 2016-11-09 中国科学院兰州化学物理研究所 A kind of high temperature resistant wide temperature range self-lubricating composite and preparation method thereof
CN106244885A (en) * 2016-07-28 2016-12-21 中国科学院兰州化学物理研究所 A kind of multiple structure aluminium oxide self-lubricating composite ceramic and preparation method thereof
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110922846A (en) * 2019-12-23 2020-03-27 山东库克斯节能环保科技有限公司 Water pump polymer super-smooth energy-saving ceramic coating material and use method thereof

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