CN103011784B - High performance nano-composite aluminum oxide based self-lubricating cutter material and preparation method thereof - Google Patents
High performance nano-composite aluminum oxide based self-lubricating cutter material and preparation method thereof Download PDFInfo
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- CN103011784B CN103011784B CN201210546512.9A CN201210546512A CN103011784B CN 103011784 B CN103011784 B CN 103011784B CN 201210546512 A CN201210546512 A CN 201210546512A CN 103011784 B CN103011784 B CN 103011784B
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Abstract
The invention relates to a high performance nano-composite aluminum oxide based self-lubricating cutter material and a preparation method thereof. The high performance nano-composite aluminum oxide based self-lubricating cutter material comprises the raw materials in percent by volume as follows: 25-55% of titanium carbide, 5-15% of nano calcium fluoride, 0.5-1.5% of magnesium oxide, and the balance of aluminum oxide. The preparation method comprises the steps: first, preparing nano calcium fluoride into a dispersing liquid; then, adding MgO, Al2O3 and TiC, mixing, dispersing, ball-grinding, drying and sieving to obtain powder; and sintering by a vacuum hot-press approach. According to the invention, nanosolid lubricant CaF3 is successfully guided into a ceramic matrix crystalline grain, so that the bending strength and hardness of the self-lubricating ceramic cutter material are improved, and the breaking tenacity is improved. The self-lubricating cutter material is low in cost of material, simple in process, small in device investment, and industrialization is easy to realize.
Description
Technical field
The present invention relates to cutter material technical field, relate in particular to high-performance nano composite alumina base self-lubricating cutter material and preparation method thereof.
Background technology
Self-lubricating knife tool refers to that cutter material itself has antifriction, wear-resistant, lubricating function, can under the condition without additional lubricating fluid or lubricant, realize self-lubricating machining, reduce facility investment, the environmental pollution of avoiding cutting fluid to cause, realization cleans production, reduce production costs, so self-lubricating knife tool is a kind of efficient, clean Green Tool, in modern machining, has broad application prospects.In stupalith, common Self-lubricating System comprises Al at present
2o
3-graphite, Al
2o
3-CaF
2and TiB
2-BN etc., the solid lubricant wherein adding in self-lubrication ceramic cutter material system is micro-meter scale.Although add the self-lubricating ceramic material tribological property of solid lubricant, be improved, due to low strength and the soft of solid lubricant, destroyed the mechanical property of material, caused the wearing quality of stupalith to reduce.
Nanotechnology is one of important channel of improving Mechanical Property of Ceramics.In self-lubrication ceramic cutter material, with the nano solid lubricant CaF of low granularity, high dispersive
2replace traditional micron self-lubricating powder, under vacuum hotpressing condition, sintering can obtain containing nano solid lubricant CaF
2novel nano self-lubrication ceramic cutter material.This technology is on the nanometer Calcium Fluoride (Fluorspan) basis of the low granularity that adopts fabrication technology to obtain, high dispersive, select suitable body material proportioning and appropriate sintering aid, and adopt rational sintering technology, the mechanical property that improves self-lubrication ceramic cutter material, acquisition can take into account the novel nano composite self-lubricating cutter material of mechanical property and tribological property.
Summary of the invention
The defect that is difficult to take into account in order to overcome existing self-lubrication ceramic cutter material mechanical property and frictional behaviour, the invention provides a kind of high-performance nano composite alumina base self-lubricating cutter material and preparation method thereof.
Summary of the invention: the present invention is by adopting nano level solid lubricant CaF
2, strong mechanical performance Al
2o
3nano-micron compound effect with TiC and sintering aid MgO, by specific sintering process, obtain adding the alumina base self-lubricating knife tool material of nano solid lubricant, optimized the mechanical property of self-lubricating knife tool material, the self-lubricating knife tool material of preparation has higher mechanical property and friction and wear behavior, in high-speed dry cutting field, has a good application prospect.
Detailed Description Of The Invention:
Technical scheme of the present invention is as follows:
A high-performance nano composite alumina base self-lubricating cutter material, raw material volume percent is composed as follows:
Titanium carbide 25-55%; Nanometer Calcium Fluoride (Fluorspan) 5-15%; Magnesium oxide 0.5-1.5%; Aluminum oxide surplus;
Described aluminum oxide micron-sized powder, being milled to median size is 1~2 μ m;
Described titanium carbide is micron-sized powder, and being milled to median size is 1~2 μ m;
Described nanometer Calcium Fluoride (Fluorspan) particle size range is 15-50nm.
Preferred according to the present invention, described high-performance nano composite alumina base self-lubricating cutter material, raw material volume percent is composed as follows:
Aluminum oxide 40-55%; Titanium carbide 30-50%; Nanometer Calcium Fluoride (Fluorspan) 5-15%; Magnesium oxide 0.5-1%.
Preferred according to the present invention, described high-performance nano composite alumina base self-lubricating cutter material, raw material volume percent is composed as follows:
Aluminum oxide 40%; Titanium carbide 49.5%; Nanometer Calcium Fluoride (Fluorspan) 10%; Magnesium oxide 0.5%.
According to the present invention, a kind of preparation method of high-performance nano composite alumina base self-lubricating cutter material, comprises that step is as follows:
(1) according to the mol ratio of 1: 2.5, take nitrocalcite and Neutral ammonium fluoride, add respectively in ethanol-distilled water mixing solutions, make the ca nitrate soln that nitrocalcite content is 1mol/L, the ammonium fluoride solution that Neutral ammonium fluoride content is 2.2-3.0mol/L.Again described ca nitrate soln and ammonium fluoride solution are added respectively to magnetic agitation 40-80min in polyoxyethylene glycol-dehydrated alcohol dispersion liquid, ultrasonic dispersion 10-30min, obtain respectively nitrocalcite dispersion liquid and Neutral ammonium fluoride dispersion liquid, by described nitrocalcite dispersion liquid and Neutral ammonium fluoride dispersion liquid, hybrid reaction 3-5min under ultrasonic and mechanical stirring condition, centrifugal, cleaning, obtain nanometer Calcium Fluoride (Fluorspan), the nanometer Calcium Fluoride (Fluorspan) making is added to the nanometer Calcium Fluoride (Fluorspan) dispersion liquid that obtains particle size range 15-50nm in polyoxyethylene glycol-dehydrated alcohol dispersion liquid;
(2) by proportioning, load weighted aluminum oxide, titanium carbide and magnesium oxide are joined successively in the nanometer Calcium Fluoride (Fluorspan) dispersion liquid of step (1), after blending dispersion 40-60min, add in ball grinder, adopt sintered carbide ball ball milling 48-72h, after vacuum-drying 24-36h, adopt 200 mesh sieves to sieve, obtain composite powder, standby;
(3) composite powder of step (2) is added in graphite jig, adopt vacuum hot pressing sintering technique, sintering under 1550 ℃-1700 ℃ of sintering temperatures and insulation 15-30min condition, naturally cooling after sintering completes.
According to aforesaid method of the present invention, preferred, in the middle ethanol-distilled water mixing solutions of step (1), the volume ratio of ethanol and distilled water is 1~3: 1~2.
According to aforesaid method of the present invention, preferred, in the described polyoxyethylene glycol-dehydrated alcohol dispersion liquid of step (1), the content of polyoxyethylene glycol is 3.5-4.5g/L.
According to aforesaid method of the present invention, preferred, in step (1), polyoxyethylene glycol-dehydrated alcohol dispersion liquid is respectively described ca nitrate soln, the 4-8 volume times of ammonium fluoride solution.
According to aforesaid method of the present invention, preferred, in the described nanometer Calcium Fluoride (Fluorspan) dispersion liquid of step (1), the content of nanometer Calcium Fluoride (Fluorspan) is 6.9-20.7g/L.
According to aforesaid method of the present invention, preferred, in step (1), polyoxyethylene glycol used is PEG6000.
According to aforesaid method of the present invention, preferred, in the described sintering process of step (3), from starting to heat up, be sintered to temperature and rise to sintering temperature and be forced into gradually 24-36MPa from normal pressure.This pressure process mean rate is 0.4~0.6MPa/min, and whole temperature-rise period continues 1 hour.
In the high-performance nano composite alumina base self-lubricating cutter material that the present invention prepares, nanometer CaF
2mainly be positioned at matrix grain inside (intracrystalline type), granularity is below 100nm.The bending strength of gained composite ceramic tool material is 600-700MPa, and fracture toughness property is 6-8.5MPam
1/2, hardness is 16-19GPa.
It is inner that the present invention introduces ceramic crystal by the solid lubricant of soft, solved the lower difficult problem of current self-lubrication ceramic cutter material comprehensive mechanical property.Do not reducing under the good rubbing characteristics prerequisite of solid lubrication agent content and maintenance, reduce the damage of solid lubricant to cutter material mechanical performance, bending strength and the hardness of self-lubrication ceramic cutter material under the effect of nanometer size effect, have been improved simultaneously, improve fracture toughness property, prepared high-performance nano composite alumina base self-lubricating cutter material.
The present invention, not reducing under the good rubbing characteristics prerequisite of solid lubrication agent content and maintenance, by nano-micron compound technology, selects suitable sintering process, by nano solid lubricant CaF
2the inside of ceramic matrix crystal grain is introduced in success, and the fracture mode of stupalith is mainly the nanocrystalline interior transgranular fracture causing mutually, has consumed a large amount of energy-to-break, has obtained and has had the self-lubricating knife tool material that higher force is learned performance.The aluminium base self-lubricating knife tool material of nano composite oxides of preparation has the advantages that mechanical property is good, self-lubricating property is good, can meet preferably the requirement of machining, and this cutter has the features such as raw material is cheap, technique is simple, equipment investment is few, be easy to realize industrialization.
Accompanying drawing explanation
Fig. 1 is the stereoscan photograph of the high-performance nano composite alumina base self-lubricating cutter material fracture of embodiment 1.
Fig. 2 is the transmission electron microscope photo of the high-performance nano composite alumina base self-lubricating cutter material of embodiment 1.
Embodiment
Below in conjunction with embodiment, the present invention will be further described.In the feed composition of each embodiment, Al used
2o
3with TiC powder, be milled to median size and be 1.5 μ m, purity is greater than 99%; CaF
2particle size range is 15-50nm.Polyoxyethylene glycol used is polyethylene glycol 6000.
Embodiment 1
High-performance nano composite alumina base self-lubricating cutter material, the volume percent of feed composition is: 40%Al
2o
3, 49.5%TiC, 10%CaF
2, 0.5%MgO.Preparation method is as follows:
(1) prepare nanometer Calcium Fluoride (Fluorspan) dispersion liquid
According to the mol ratio ratio of 1: 2.5, take respectively nitrocalcite 4.72g and Neutral ammonium fluoride 1.85g, put into separately beaker, respectively add respectively 10ml distilled water and 10ml dehydrated alcohol, shake up dissolving, obtain pre-assigned nitrocalcite and ammonium fluoride solution; Take the PEG6000 of 0.8g, add in 200ml dehydrated alcohol, ultrasonic dispersion 20min, dissolves it completely, obtains the double solvents of polyoxyethylene glycol and dehydrated alcohol.The double solvents equivalent that this is prepared is divided into two parts, adds respectively in pre-assigned nitrocalcite and ammonium fluoride solution magnetic agitation 60min, ultrasonic dispersion 20min; Obtain scattered ca nitrate soln and ammonium fluoride solution.Under ultrasonic and agitation condition, scattered ca nitrate soln is poured in scattered ammonium fluoride solution into reaction 3min.Take out reacted solution, place ageing 48h.Under 4000r/min condition, carry out centrifugation 30min, with dehydrated alcohol, clean 5 times, obtain the CaF that median size is 20.4nm
2, the content that adds polyoxyethylene glycol is 4g/L polyoxyethylene glycol-dehydrated alcohol dispersion liquid, makes CaF
2content is the nanometer CaF of 13.8g/L
2dispersion liquid.
(2) by proportioning, by Al
2o
3, TiC and MgO add CaF successively
2in dispersion liquid, blending dispersion 40min under ultrasonic wave and mechanical stirring, then adopts sintered carbide ball ball milling 48h, adopts 200 order sub-sieves to sieve after vacuum-drying 24h;
(3) composite powder is added in graphite jig, adopt vacuum hot pressing sintering technique, sintering under 1650 ℃ of sintering temperatures and insulation 15min condition, pressurization gradually after sintering starts, when temperature rises to sintering temperature, pressure reaches 30MPa, this pressure process mean rate is 0.5MPa/min, and whole temperature-rise period continues 1 hour.Naturally cooling after sintering completes.
The stupalith sample making is carried out to cutting processing, record its mechanical property parameters and be: bending strength 655MPa, fracture toughness property 8.25MPam
1/2, Vickers' hardness 18.68GPa.The stereoscan photograph of Fig. 1 shows that nanometer Calcium Fluoride (Fluorspan) is evenly distributed in ceramic matrix, and without reuniting, the fracture mode of material be take transgranular fracture as main.The transmission electron microscope photo of Fig. 2 shows that Calcium Fluoride (Fluorspan) is mainly positioned at matrix grain inside, and granularity is between 40-100nm, and after sintering, crystal grain does not occur obviously to grow up.
Embodiment 2
High-performance nano composite alumina base self-lubricating cutter material, the volume percent of feed composition is: 59%Al
2o
3, 30%TiC, 10%CaF
2, 1%MgO.Preparation method is as follows:
(1) prepare nanometer Calcium Fluoride (Fluorspan) dispersion liquid as embodiment 1.
(2) by load weighted Al
2o
3, TiC and MgO add in mother liquor successively, blending dispersion 60min under ultrasonic wave and mechanical stirring, then adopts sintered carbide ball ball milling 72h, adopts 200 order sub-sieves to sieve after vacuum-drying 36h;
(3) composite powder is added in graphite jig, adopt vacuum hot pressing sintering technique, sintering under 1550 ℃ of sintering temperatures and insulation 30min condition, in sintering process, with temperature, raise and tune up gradually pressure, when temperature rises to sintering temperature, pressure reaches 25MPa, this pressure process mean rate is about 0.417MPa/min, and whole temperature-rise period continues 1 hour.Naturally cooling after sintering completes.
The stupalith sample making is carried out to cutting processing, record its mechanical property parameters and be: bending strength 674MPa, fracture toughness property 6.42MPam
1/2, Vickers' hardness 16.16GPa.
Embodiment 3
High-performance nano composite alumina base self-lubricating cutter material, the volume percent of feed composition is: 42%Al
2o
3, 42%TiC, 15%CaF
2, 1%MgO.Preparation method is as follows:
(1) prepare nanometer Calcium Fluoride (Fluorspan) dispersion liquid
According to the mol ratio ratio of 1: 2.5, take respectively nitrocalcite 7.08g and Neutral ammonium fluoride 2.78g, put into separately beaker, respectively add respectively 15ml distilled water and 10ml dehydrated alcohol, shake up dissolving, obtain pre-assigned nitrocalcite and ammonium fluoride solution; Take the PEG6000 of 0.8g, add in 200ml dehydrated alcohol, ultrasonic dispersion 20min, dissolves it completely, obtains the double solvents of polyoxyethylene glycol and dehydrated alcohol.The double solvents equivalent that this is prepared is divided into two parts, adds respectively in pre-assigned nitrocalcite and ammonium fluoride solution magnetic agitation 80min, ultrasonic dispersion 30min; Obtain scattered ca nitrate soln and ammonium fluoride solution.Under ultrasonic and agitation condition, scattered ca nitrate soln is poured in scattered ammonium fluoride solution into reaction 5min.Take out reacted solution, place ageing 48h.Under 4000r/min condition, carry out centrifugation 30min, with dehydrated alcohol, clean 5 times, obtain the CaF that median size is 20.4nm
2, the content that adds polyoxyethylene glycol is 5g/L polyoxyethylene glycol-dehydrated alcohol dispersion liquid, makes CaF
2content is the nanometer CaF of 20.7g/L
2dispersion liquid.
(2) by load weighted Al
2o
3, TiC and MgO add in mother liquor successively, blending dispersion 40min under ultrasonic wave and mechanical stirring, then adopts sintered carbide ball ball milling 48h, adopts 200 order sub-sieves to sieve after vacuum-drying 24h;
(3) composite powder is added in graphite jig, adopt vacuum hot pressing sintering technique, sintering under 1600 ℃ of sintering temperatures and insulation 20min condition, in sintering process, with temperature, raise and tune up gradually pressure, pressurization gradually after sintering starts, when temperature rises to sintering temperature, pressure reaches 24MPa, and this pressure process mean rate is about 0.4MPa/min, and whole temperature-rise period continues 1 hour.Naturally cooling after sintering completes.
The stupalith sample making is carried out to cutting processing, record its mechanical property parameters and be: bending strength 612MPa, fracture toughness property 6.53MPam
1/2, Vickers' hardness 16.2GPa.
Embodiment 4
High-performance nano composite alumina base self-lubricating cutter material, the volume percent of feed composition is: 44.5%Al
2o
3, 49%TiC, 5%CaF
2, 1.5%MgO.Preparation method is as follows:
According to the mol ratio ratio of 1: 2.5, take respectively nitrocalcite 2.36g and Neutral ammonium fluoride 0.93g, preparation nanometer Calcium Fluoride (Fluorspan) dispersion liquid, as embodiment 1, makes CaF
2content is the nanometer CaF of 6.9g/L
2dispersion liquid.
By load weighted Al
2o
3, TiC and MgO add in nanometer Calcium Fluoride (Fluorspan) dispersion liquid (embodiment 1 step (1) makes) successively, blending dispersion 50min under ultrasonic wave and mechanical stirring, then adopts sintered carbide ball ball milling 48h, adopts 200 order sub-sieves to sieve after vacuum-drying 36h; Composite powder is added in graphite jig, adopt vacuum hot pressing sintering technique, sintering under 1650 ℃ of sintering temperatures and insulation 30min condition, in sintering process, with temperature, raise and tune up gradually pressure, pressurization gradually after sintering starts, when temperature rises to sintering temperature, pressure reaches 36MPa, and this pressure process mean rate is about 0.6MPa/min, and whole temperature-rise period continues 1 hour.Naturally cooling after sintering completes.The stupalith sample making is carried out to cutting processing, record its mechanical property parameters and be: bending strength 688MPa, fracture toughness property 6.36MPam
1/2, Vickers' hardness 18.47GPa.
Comparative example: the alumina base self-lubricating knife tool material that adds micron Calcium Fluoride (Fluorspan) solid lubricant
As the formula of embodiment 1, difference is to adopt commercially available micron order CaF
2as solid lubricant.
The alumina base self-lubricating knife tool material that adds micron Calcium Fluoride (Fluorspan) solid lubricant, the volume percent of feed composition is: 40%Al
2o
3, 49.5%TiC, 10% micron of CaF
2, 0.5%MgO.Preparation process is as follows:
By proportioning, by Al
2o
3, TiC, micron CaF
2add successively in polyoxyethylene glycol dispersion liquid with MgO, blending dispersion 40min under ultrasonic wave and mechanical stirring, then adopts sintered carbide ball ball milling 48h, adopts 200 order sub-sieves to sieve after vacuum-drying 24h; Gained composite powder is added in graphite jig, adopt vacuum hot pressing sintering technique, sintering under 1650 ℃ of sintering temperatures and insulation 15min condition, pressurization gradually after sintering starts, when temperature rises to sintering temperature, pressure reaches 30MPa, this pressure process mean rate is 0.5MPa/min, and whole temperature-rise period continues 1 hour.Naturally cooling after sintering completes.The stupalith sample making is carried out to cutting processing, record its mechanical property parameters and be: bending strength 528MPa, fracture toughness property 4.45MPam
1/2, Vickers' hardness 15.2GPa.
Claims (4)
1. a preparation method for the aluminium base self-lubricating knife tool material of nano composite oxides, raw material volume percent is composed as follows:
Titanium carbide 25-55%; Nanometer Calcium Fluoride (Fluorspan) 5-15%; Magnesium oxide 0.5-1.5%; Aluminum oxide surplus;
Described aluminum oxide is micron-sized powder, and being milled to median size is 1 ~ 2 μ m;
Described titanium carbide is micron-sized powder, and being milled to median size is 1 ~ 2 μ m;
Described nanometer Calcium Fluoride (Fluorspan) particle size range is 15-50nm;
Preparation process is as follows:
(1) according to the mol ratio of 1:2.5, take nitrocalcite and Neutral ammonium fluoride, add respectively in ethanol-distilled water mixing solutions, make the ca nitrate soln that nitrocalcite content is 1mol/L, the ammonium fluoride solution that Neutral ammonium fluoride content is 2.2-3.0mol/L, again described ca nitrate soln and ammonium fluoride solution are added respectively to magnetic agitation 40-80min in polyoxyethylene glycol-dehydrated alcohol dispersion liquid, ultrasonic dispersion 10-30min, polyoxyethylene glycol-dehydrated alcohol dispersion liquid used is respectively described ca nitrate soln, the 4-8 volume of ammonium fluoride solution doubly, obtain respectively nitrocalcite dispersion liquid and Neutral ammonium fluoride dispersion liquid, by described nitrocalcite dispersion liquid and Neutral ammonium fluoride dispersion liquid, hybrid reaction 3-5min under ultrasonic and mechanical stirring condition, centrifugal, clean, obtain nanometer Calcium Fluoride (Fluorspan), the nanometer Calcium Fluoride (Fluorspan) making is added to the nanometer Calcium Fluoride (Fluorspan) dispersion liquid that obtains particle size range 15-50nm in polyoxyethylene glycol-dehydrated alcohol dispersion liquid,
In described nanometer Calcium Fluoride (Fluorspan) dispersion liquid, the content of nanometer Calcium Fluoride (Fluorspan) is 6.9-20.7g/L;
In described ethanol-distilled water mixing solutions, the volume ratio of ethanol and distilled water is 1 ~ 3:1 ~ 2;
In described polyoxyethylene glycol-dehydrated alcohol dispersion liquid, the content of polyoxyethylene glycol is 3.5-4.5g/L;
(2) by proportioning, load weighted aluminum oxide, titanium carbide and magnesium oxide are joined successively in the nanometer Calcium Fluoride (Fluorspan) dispersion liquid of step (1), after blending dispersion 40-60min, add in ball grinder, adopt sintered carbide ball ball milling 48-72h, after vacuum-drying 24-36h, adopt 200 mesh sieves to sieve, obtain composite powder, standby;
(3) composite powder of step (2) is added in graphite jig, adopt vacuum hot pressing sintering technique, sintering under 1550 ℃-1700 ℃ of sintering temperatures and insulation 15-30min condition, naturally cooling after sintering completes.
2. the aluminium base self-lubricating knife tool material of nano composite oxides as claimed in claim 1, is characterized in that, raw material volume percent is composed as follows:
Aluminum oxide 40-55%; Titanium carbide 30-50%; Nanometer Calcium Fluoride (Fluorspan) 5-15%; Magnesium oxide 0.5-1%.
3. the aluminium base self-lubricating knife tool material of nano composite oxides as claimed in claim 1, is characterized in that, raw material volume percent is composed as follows:
Aluminum oxide 40%; Titanium carbide 49.5%; Nanometer Calcium Fluoride (Fluorspan) 10%; Magnesium oxide 0.5%.
4. the preparation method of the aluminium base self-lubricating knife tool material of nano composite oxides as claimed in claim 1, is characterized in that, in step (1), polyoxyethylene glycol used is PEG6000.
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CN104045351B (en) * | 2014-06-26 | 2015-07-08 | 齐鲁工业大学 | Aluminum oxide coated calcium fluoride powder for self-lubricating cutter material and preparation method of powder |
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CN104387041A (en) * | 2014-11-11 | 2015-03-04 | 合肥皖为电气设备工程有限责任公司 | Aluminum oxide ceramic for self-lubricated cutter and preparation method of aluminum oxide ceramic |
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CN104844178B (en) * | 2015-06-08 | 2016-09-21 | 齐鲁工业大学 | Add the preparation method of the self-lubrication ceramic cutter material of spherical nano-silicon dioxide cladding hexagonal boron nitride composite granule |
CN104962110B (en) * | 2015-07-02 | 2017-05-03 | 齐鲁工业大学 | Nickel-boron-coating calcium fluoride composite powder, preparation and application thereof and self-lubricating ceramic cutter |
CN115321991B (en) * | 2021-05-11 | 2023-05-05 | 中国科学院过程工程研究所 | Method for preparing self-lubricating material by utilizing aluminum ash |
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