CN104892005A - Preparation method of silicon nitride-based self-lubricating ceramic cutter material containing alumina-coated hexagonal boron nitride composite powder - Google Patents
Preparation method of silicon nitride-based self-lubricating ceramic cutter material containing alumina-coated hexagonal boron nitride composite powder Download PDFInfo
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Abstract
The invention relates to a preparation method of a silicon nitride-based self-lubricating ceramic cutter material containing alumina-coated hexagonal boron nitride composite powder. The silicon nitride-based self-lubricating ceramic cutter material comprises, by volume, 57-70% of micrometer silicon nitride, 5-15% of nanometer silicon nitride, 5-15% of micrometer titanium carbide, 3.2% of alumina, 4.8% of yttrium oxide, and 2-15% of alumina-coated hexagonal boron nitride. The preparation method comprises preparing alumina-coated hexagonal boron nitride composite powder with particle sizes of 4-12 micrometers, weighing micrometer silicon nitride, nanometer silicon nitride and micrometer titanium carbide, respectively preparing their suspension liquids, carrying out ultrasonic dispersion, carrying out mixing, adding alumina and yttrium oxide into the mixture, carrying out ultrasonic dispersion for 15-20min to obtain a composite suspension liquid, carrying out ball milling, adding the alumina-coated hexagonal boron nitride composite powder into the composite suspension liquid, carrying out ball milling, carrying out vacuum drying to obtain mixed powder and carrying out vacuum hot pressing sintering molding. The silicon nitride-based self-lubricating ceramic cutter material containing alumina-coated hexagonal boron nitride composite powder can improve ceramic cutter mechanical properties and guarantee self-lubricating performances.
Description
Technical field
The present invention relates to a kind of preparation method of nitride silicon based self-lubrication ceramic cutter material, particularly add the nitride silicon based self-lubrication ceramic cutter material preparation method of alumina-coated hexagonal boron nitride composite powder, belong to self-lubricating knife tool field of material technology.
Background technology
In metal cutting process, the negative effect that the use of cutting fluid brings is more and more obvious, contaminate environment, harm workman process that is healthy, cutting fluid increase the production cost etc. of enterprise, and therefore, cancellation cutting fluid replaces Dry-cutting and can solve the problem well.There has been proposed the concept of self-lubricating knife tool thus, add in cutter by solid lubricant, allow solid lubricant Dispersed precipitate in cutter, make cutter have self-lubricating property, reduce frictional coefficient, and reduce the wearing and tearing of cutter, improve cutting-tool's used life.Research finds the composite self-lubricating cutter material be prepared into containing solid lubricant, and along with the increase of solid lubrication agent content, the mechanical property of self-lubricating knife tool material generally reduces with the increase of lubricant content.
Hexagonal boron nitride (h-BN) has very excellent chemical stability, and still very stable at the temperature of 2800 DEG C in an inert atmosphere, also having good lubricity, is a kind of excellent solid lubricant.In ceramic cutting tool material, add h-BN, effectively can improve lubricity and the thermal shock resistance of stupalith, realize the effect of antifriction antiwear, avoid the environment and Cost Problems that use lubricating fluid to bring.But the mechanical property of h-BN is lower, in cutter, Dispersed precipitate likely makes the mechanical degradation of cutter.For overcoming this shortcoming, people develop micro-chamber self-lubricating knife tool, coating self-lubricating knife tool and reaction in－situ self-lubricating knife tool.But these three kinds of methods all do not have fundamentally to solve the problem of directly adding solid lubricant and causing cutter mechanical property to reduce in cutter.CN102502535A discloses a kind of method preparing the coated hexagonal boron nitride of charcoal, for hexagonal boron nitride prepared by raw material with boric acid and urea, again with maleic anhydride ethylene octene graft copolymer for carbon source, by stirring, extraction, suction filtration, drying and high temperature cabonization step, obtain the coated hexagonal boron nitride of charcoal of nucleocapsid structure; Add in base oil or macromolecule resin and show good dispersiveness, and still can show good mechanical property and good wear resisting property at the extreme environment such as high temperature, high pressure.But this charcoal coated hexagonal boron nitride method be not suitable for nitride silicon based self-lubrication ceramic cutter material.
Summary of the invention
In order to make up the deficiencies in the prior art, a kind of preparation method adding the nitride silicon based self-lubrication ceramic cutter material of alumina-coated hexagonal boron nitride composite powder is provided, both ensured the mechanical property of self-lubricating knife tool and taken into account its self-lubricating property, make the Vickers' hardness of cutter material, fracture toughness property, bending strength improve and anti-attrition wear resisting property is better.
Technical scheme of the present invention is as follows:
Add a preparation method for the nitride silicon based self-lubrication ceramic cutter material of alumina-coated hexagonal boron nitride composite powder, feed composition volume percent is: micron silicon nitride (α-Si
3n
4) 57-70%, nano-silicon nitride (α-Si
3n
4) 5-15%, micrometer silicon carbide titanium 5-15%, aluminum oxide 3.2%, yttrium oxide 4.8%, alumina-coated hexagonal boron nitride 2-15%;
Comprise step as follows:
(1) hexagonal boron nitride powder and the dispersion agent polyoxyethylene glycol of getting particle diameter 3-10 μm are mixed in the hexagonal boron nitride suspension that distilled water is made into 3-8g/L, and dispersion agent addition is the 3-5% of hexagonal boron nitride quality.Add acetic acid-sodium acetate buffer solution that pH value is 4.5, ultrasonic disperse is also stirred and heated to 30 DEG C-40 DEG C, slowly drips Al
3+concentration is the aluminum nitrate solution of 0.1-0.2mol/L, the add-on of described aluminum nitrate solution is according to mol ratio BN: Al=1: 0.5-1 meter, slowly dripping ammoniacal liquor to reacting liquid pH value is again 7.0-7.5, dropwise and keep temperature 30 DEG C-40 DEG C reaction 1.5-2.5h, then still aging, sedimentation and filtration, cleaning, the hexagonal boron nitride composite powder that centrifugal, vacuum-drying obtains Surface coating aluminium hydroxide, through vacuum calcining, the alumina-coated hexagonal boron nitride composite powder of obtained particle diameter 4-12 μm;
(2) in proportion, a micron silicon nitride is taken respectively, nano-silicon nitride, micrometer silicon carbide titanium, with appropriate dehydrated alcohol for dispersion medium, be configured to a micron silicon nitride, micrometer silicon carbide titanium suspension and nano silicon nitride silicon suspension respectively, ultrasonic disperse 15-20min while of well-beaten; Scattered micron silicon nitride, micrometer silicon carbide titanium suspension and nano silicon nitride silicon suspension are mixed, then adds described aluminum oxide, yttrium oxide in proportion, fully stir and ultrasonic disperse 15-20min; Obtain complex phase suspension;
(3) above-mentioned complex phase suspension is poured in ball grinder, be filled with argon gas or nitrogen as shielding gas, add ball milling ball, ball milling 36-48h, mixture after ball milling, taking the alumina-coated hexagonal boron nitride composite powder of step (1) in proportion, take dehydrated alcohol as dispersion medium, be made into suspension, ultrasonic disperse 10min; Gained suspension is added in the mixture after ball milling, is filled with argon gas or nitrogen as shielding gas, adds ball milling ball, continue ball milling 8-12h.Then take out ball milling liquid and be placed in loft drier, vacuum-drying 24-36h under 100-120 DEG C of condition; After drying completely, gained mixed powder is crossed 200 mesh sieves, obtain mixed powder, seal for subsequent use;
(4) vacuum hot-pressed sintered technology is adopted, the mixed powder pressing mold sinter molding obtained by step (3).
According to preferred for this invention, described feed composition volume percent is micron silicon nitride 62-67%, nano-silicon nitride 10%, micrometer silicon carbide titanium 10%, aluminum oxide 3.2%, yttrium oxide 4.8%, alumina-coated hexagonal boron nitride 5-10%.The cutter material comprehensive mechanical property adopting this proportioning to prepare and properties of antifriction and wear resistance best.
Preferred according to the present invention, the stirring heating described in step (1) is magnetic agitation heating in digital display heat-collecting magnetic stirring device, and suspension is uniformly dispersed.
Preferred according to the present invention, aluminum nitrate solution described in step (1) is that nine water aluminum nitrates add water preparation; Most preferably Al
3+concentration is the aluminum nitrate solution of 0.15mol/L.
Preferred according to the present invention, described in step (1), pH buffered soln addition is 8-15mL/100mL distilled water, and preferably pH buffered soln addition is 10-11mL/100mL distilled water further.
Preferred according to the present invention, the ammoniacal liquor described in step (1), is be 28% strong aqua distilled water diluting 5-10 times by mass percent, obtains the ammonia soln that pH value is 6.5-8.5.
Preferred according to the present invention, the suspension described in step (1) is still aging, is suspension is carried out standing 10-12 hour, and reactant is fully precipitated; Distilled water wash 2-3 time, absolute ethanol washing 2-3 time are used in described washing respectively.
Preferred according to the present invention, vacuum calcining described in step (1), be by drying completely the coated hexagonal boron nitride composite powder of aluminium hydroxide be placed in alumina crucible, vacuum calcining in vacuum sintering funace, temperature rise rate is 8-12 DEG C/min, sintering temperature is 1100-1200 DEG C, and soaking time is 1.5-2.5h, obtained alumina-coated hexagonal boron nitride composite powder.
Preferred according to the present invention, in step (2), micron silicon nitride median size (D50) is 0.5 μm, nano-silicon nitride median size (D50) is 50nm, micrometer silicon carbide titanium median size (D50) is 0.5 μm, aluminum oxide median size (D50) is 1 μm, yttrium oxide median size (D50) is 1 μm, and raw material is commercially available prod.
Preferred according to the present invention, the ball milling ball described in step (3) is Wimet (YG8) ball.The addition of ball milling ball is 10 times of each component raw material total mass.Described in step (3), loft drier is electric vacunm drying case.
Preferred according to the present invention, vacuum hot-pressed sintered technology in described step (4), be first load in graphite jig by powder, coldmoulding 15min carries out hot pressed sintering again.Preferably hot pressed sintering parameter is further: hot pressed sintering temperature 1650-1700 DEG C, soaking time 45-75min, pressure 25-30MPa, temperature rise rate 10-20 DEG C/min.
The ceramic body that described step (4) hot pressed sintering is prepared, is prepared into the ceramic batten of 3mm × 4mm × 30mm through cutting processing-corase grind-fine grinding-grinding-polishing step.
The present invention adopts heterogeneous nucleation process, first aluminium hydroxide is coated to hexagonal boron nitride particles surface, makes the coated hexagonal boron nitride composite powder of aluminium hydroxide, then prepares alumina-coated hexagonal boron nitride composite powder by vacuum calcining.This alumina-coated hexagonal boron nitride composite powder is added in nitride silicon based self-lubrication ceramic cutter material, with micron silicon nitride for matrix, interpolation micrometer silicon carbide titanium and nano-silicon nitride are as wild phase, with micrometer alumina and micron yttrium oxide for sintering aid, alumina-coated hexagonal boron nitride composite powder is as self-lubricating phase, make self-lubrication ceramic cutter material through vacuum heating-press sintering, the mechanical property of sintex can be improved, its self-lubricating function can be taken into account simultaneously.Compared with the nitride silicon based self-lubricating knife tool material added without the h-BN of Surface coating process, the nitride silicon based self-lubrication ceramic cutter material adding 10vol.% cladded type solid lubricant h-BN improves 27%, 22.2% and 5.9% respectively in Vickers' hardness, fracture toughness property and bending strength, and mechanical property significantly improves.
Accompanying drawing explanation
Fig. 1 is alumina-coated hexagonal boron nitride powder particle surface SEM surface topography map.
Fig. 2 is the SEM shape appearance figure after embodiment 1 adds the test sample surface corrosion of the self-lubricating knife tool material of cladded type hexagonal boron nitride composite powder.
Fig. 3 is the test sample surface of fracture SEM shape appearance figure that embodiment 1 adds the self-lubricating knife tool material of cladded type hexagonal boron nitride composite powder.
Embodiment
Below in conjunction with specific embodiment, the present invention is further elaborated, but the present invention is not limited in following examples.Described method is ordinary method if no special instructions.
The alumina-coated hexagonal boron nitride composite powder used in each embodiment component obtains by the following method:
Take 0.5g hexagonal boron nitride powder and the dispersion agent polyethylene glycol 6000 accounting for hexagonal boron nitride powder quality 4% respectively, be mixed in 100ml distilled water and be configured to suspension.In suspension, add the buffered soln 10mL that pH is 4.5, ultrasonic disperse 10min, and in digital display heat-collecting magnetic stirring device magnetic agitation be heated to 35 DEG C.Take nine appropriate water aluminum nitrates, be configured to the aluminum nitrate solution of 0.15mol/L concentration, in instillation hexagonal boron nitride suspension, again by be diluted to concentration be 2.5% ammoniacal liquor slowly instill in suspension, temperature of reaction is 35 DEG C, until the pH value of suspension reaches 7.5, continues reaction stirring 2 hours.Obtained suspension is left standstill 12 hours, and filtering-depositing, respectively washes 2 times with distilled water and dehydrated alcohol, with supercentrifuge with the centrifugal 10min of 2000r/min, is then placed in loft drier, dry 24h under 80 DEG C of conditions.The obtained coated hexagonal boron nitride composite powder of aluminium hydroxide.By drying completely the coated hexagonal boron nitride composite powder of aluminium hydroxide be placed in crucible, adopt vacuum sintering funace carry out vacuum calcining.The temperature of vacuum calcining is 1200 DEG C, and temperature rise rate is 10 DEG C/min, insulation 2h.Final obtained alumina-coated hexagonal boron nitride composite powder.As shown in Figure 1, median size is 5 μm to pattern.
Micron silicon nitride median size (D50) used in embodiment is 0.5 μm, nano-silicon nitride median size (D50) is 50nm, micrometer silicon carbide titanium median size (D50) is 0.5 μm, aluminum oxide median size (D50) is 1 μm, yttrium oxide median size (D50) is 1 μm, and raw material is commercially available prod.
Ball milling ball used in embodiment is Wimet (YG8) ball.Loft drier used is electric vacunm drying case.
Embodiment 1
The each feed composition volume percent of nitride silicon based self-lubrication ceramic cutter material of adding alumina-coated hexagonal boron nitride composite powder is micron silicon nitride (α-Si
3n
4) 62%, nano-silicon nitride (α-Si
3n
4) 10%, micrometer silicon carbide titanium 10%, aluminum oxide 3.2%, yttrium oxide 4.8%, alumina-coated hexagonal boron nitride 10%.
In proportion, a micron silicon nitride (α-Si is taken respectively
3n
4), nano-silicon nitride (α-Si
3n
4), micrometer silicon carbide titanium, aluminum oxide, yttrium oxide.With appropriate dehydrated alcohol for dispersion medium, be configured to a micron silicon nitride, micrometer silicon carbide titanium suspension and nano silicon nitride silicon suspension respectively, ultrasonic disperse 15min while of well-beaten.Gained micron silicon nitride, micrometer silicon carbide titanium suspension and nano silicon nitride silicon suspension are mixed, then aluminum oxide and yttrium oxide are added obtained mixing suspension, fully stir and ultrasonic disperse 15min.
Above-mentioned complex phase suspension is poured in ball grinder, is filled with nitrogen as shielding gas, add each component raw material total mass and ball milling ball weight than the ball milling ball for 1:10, ball milling 36h, obtain mixture after ball milling.Take alumina-coated hexagonal boron nitride composite powder in proportion, add appropriate dehydrated alcohol and be made into suspension as dispersion medium, ultrasonic disperse 10min.In the mixture obtained after above-mentioned gained suspension is added ball milling, be filled with nitrogen as shielding gas, add each component raw material total amount with ball milling ball weight than the ball milling ball for 1:10, continuation ball milling 12h.Taking-up is placed in loft drier, vacuum-drying 36h under 100-120 DEG C of condition.After drying completely, mixed powder is crossed 200 mesh sieves, mixed powder is loaded in graphite jig and carry out vacuum heating-press sintering after coldmoulding 15min.Hot pressed sintering parameter is: hot pressed sintering temperature 1700 DEG C, soaking time 60min, pressure 30MPa, temperature rise rate 20 DEG C/min.Obtained nitride silicon based self-lubrication ceramic cutter material.
The ceramic body that hot pressed sintering is prepared is prepared into the ceramic batten of 3mm × 4mm × 30mm through cutting processing-corase grind-fine grinding-grinding-polishing step.Recording its mechanical property parameters is: Vickers' hardness 14.1GPa, fracture toughness property 7.2MPam
1/2, bending strength 732MPa.When joining pair with 45 steel, frictional coefficient is 0.31.
After the nitride silicon based self-lubrication ceramic cutter material processing sample surface corrosion of obtained interpolation alumina-coated hexagonal boron nitride composite powder, SEM pattern as shown in Figure 2, α-Si
3n
4β-Si is converted into through hot pressed sintering
3n
4, the β-Si in material
3n
4crisscross, in mutually nested long column shape interlocking structure, length-to-diameter ratio comparatively large (being about 3-8).By sample section SEM morphology observation in Fig. 3, there is the hole stayed after crystal grain is extracted in incision position, and thick uniform crystal particles is distributed between columnar shape basal crystal grain, and material microstructure is comparatively fine and close.
Embodiment 2
Add the nitride silicon based self-lubrication ceramic cutter of alumina-coated hexagonal boron nitride powder, each feed composition volume percent is micron silicon nitride (α-Si
3n
4) 67%, nano-silicon nitride (α-Si
3n
4) 10%, micrometer silicon carbide titanium 10%, aluminum oxide 3.2%, yttrium oxide 4.8%, alumina-coated hexagonal boron nitride 5%.
In proportion, a micron silicon nitride (α-Si is taken respectively
3n
4), nano-silicon nitride (α-Si
3n
4), micrometer silicon carbide titanium, aluminum oxide, yttrium oxide.With appropriate dehydrated alcohol for dispersion medium, be configured to a micron silicon nitride, micrometer silicon carbide titanium suspension and nano silicon nitride silicon suspension respectively, ultrasonic disperse 15min while of well-beaten.Gained micron silicon nitride, micrometer silicon carbide titanium suspension and nano silicon nitride silicon suspension are mixed, then aluminum oxide and yttrium oxide are added obtained mixing suspension, fully stir and ultrasonic disperse 15min.
Above-mentioned complex phase suspension is poured in ball grinder, is filled with nitrogen as shielding gas, add each component raw material total mass and ball milling ball weight than the ball milling ball for 1:10, ball milling 36h, obtain mixture after ball milling.Take alumina-coated hexagonal boron nitride composite powder in proportion, add appropriate dehydrated alcohol and be made into suspension as dispersion medium, ultrasonic disperse 10min.In the mixture obtained after above-mentioned gained suspension is added ball milling, be filled with nitrogen as shielding gas, add each component raw material total amount with ball milling ball weight than the ball milling ball for 1:10, continuation ball milling 12h.Taking-up is placed in loft drier, vacuum-drying 36h under 100-120 DEG C of condition.After drying completely, mixed powder is crossed 200 mesh sieves, mixed powder is loaded in graphite jig and carry out vacuum heating-press sintering after coldmoulding 15min.Hot pressed sintering parameter is: hot pressed sintering temperature 1700 DEG C, soaking time 60min, pressure 30MPa, temperature rise rate 20 DEG C/min.Obtained nitride silicon based self-lubrication ceramic cutter material.
The ceramic body that hot pressed sintering is prepared is prepared into the ceramic batten of 3mm × 4mm × 30mm through cutting processing-corase grind-fine grinding-grinding-polishing step.Recording its mechanical property parameters is: Vickers' hardness 13.3GPa, fracture toughness property 7.53MPam
1/2, bending strength 839MPa.When joining pair with 45 steel, frictional coefficient is 0.37.
Embodiment 3
The each feed composition volume percent of nitride silicon based self-lubrication ceramic cutter of adding alumina-coated hexagonal boron nitride powder is micron silicon nitride (α-Si
3n
4) 57%, nano-silicon nitride (α-Si
3n
4) 10%, micrometer silicon carbide titanium 10%, aluminum oxide 3.2%, yttrium oxide 4.8%, alumina-coated hexagonal boron nitride 15%.
In proportion, a micron silicon nitride (α-Si is taken respectively
3n
4), nano-silicon nitride (α-Si
3n
4), micrometer silicon carbide titanium, aluminum oxide, yttrium oxide.With appropriate dehydrated alcohol for dispersion medium, be configured to a micron silicon nitride, micrometer silicon carbide titanium suspension and nano silicon nitride silicon suspension respectively, ultrasonic disperse 15min while of well-beaten.Gained micron silicon nitride, micrometer silicon carbide titanium suspension and nano silicon nitride silicon suspension are mixed, then aluminum oxide and yttrium oxide are added obtained mixing suspension, fully stir and ultrasonic disperse 15min.
Above-mentioned complex phase suspension is poured in ball grinder, is filled with nitrogen as shielding gas, add each component raw material total mass and ball milling ball weight than the ball milling ball for 1:10, ball milling 36h, obtain mixture after ball milling.Take alumina-coated hexagonal boron nitride composite powder in proportion, add appropriate dehydrated alcohol and be made into suspension as dispersion medium, ultrasonic disperse 10min.In the mixture obtained after above-mentioned gained suspension is added ball milling, be filled with nitrogen as shielding gas, add each component raw material total amount with ball milling ball weight than the ball milling ball for 1:10, continuation ball milling 12h.Taking-up is placed in loft drier, vacuum-drying 36h under 100-120 DEG C of condition.After drying completely, mixed powder is crossed 200 mesh sieves, mixed powder is loaded in graphite jig and carry out vacuum heating-press sintering after coldmoulding 15min.Hot pressed sintering parameter is: hot pressed sintering temperature 1700 DEG C, soaking time 60min, pressure 30MPa, temperature rise rate 20 DEG C/min.Obtained nitride silicon based self-lubrication ceramic cutter material.
The ceramic body that hot pressed sintering is prepared is prepared into the ceramic batten of 3mm × 4mm × 30mm through cutting processing-corase grind-fine grinding-grinding-polishing step.Recording its mechanical property parameters is: Vickers' hardness 10.3GPa, fracture toughness property 6.2MPam
1/2, bending strength 637MPa.When joining pair with 45 steel, frictional coefficient is 0.42.
Embodiment 4: comparative example
The each feed composition volume percent of nitride silicon based self-lubrication ceramic cutter of adding the not coated hexagonal boron nitride powder in surface is micron silicon nitride (α-Si
3n
4) 62%, nano-silicon nitride (α-Si
3n
4) 10%, micrometer silicon carbide titanium 10%, aluminum oxide 3.2%, yttrium oxide 4.8%, the hexagonal boron nitride 10% that surface is not coated.
In proportion, a micron silicon nitride (α-Si is taken respectively
3n
4), nano-silicon nitride (α-Si
3n
4), micrometer silicon carbide titanium, aluminum oxide, yttrium oxide.With appropriate dehydrated alcohol for dispersion medium, be configured to a micron silicon nitride, micrometer silicon carbide titanium suspension and nano silicon nitride silicon suspension respectively, ultrasonic disperse 15min while of well-beaten.Gained micron silicon nitride, micrometer silicon carbide titanium suspension and nano silicon nitride silicon suspension are mixed, then aluminum oxide and yttrium oxide are added obtained mixing suspension, fully stir and ultrasonic disperse 15min.
Above-mentioned complex phase suspension is poured in ball grinder, is filled with nitrogen as shielding gas, add the ball milling ball that each component raw material total amount is 1:10 with ball milling ball weight ratio, take out after ball milling 36h.Take the hexagonal boron nitride powder (median size is 5 μm) that surface is not coated in proportion, add appropriate dehydrated alcohol and be made into suspension as dispersion medium, ultrasonic disperse 10min, mixes.In the mixture obtained after above-mentioned gained suspension is added ball milling, be filled with nitrogen as shielding gas, add each component raw material total amount with ball milling ball weight than the ball milling ball for 1:10, continuation ball milling 12h.Taking-up is placed in loft drier, vacuum-drying 36h under 100-120 DEG C of condition.After drying completely, mixed powder is crossed 200 mesh sieves, mixed powder is loaded in graphite jig and carry out vacuum heating-press sintering after coldmoulding 15min.Hot pressed sintering parameter is: hot pressed sintering temperature 1700 DEG C, soaking time 60min, pressure 30MPa, temperature rise rate 20 DEG C/min.The obtained nitride silicon based self-lubrication ceramic cutter material adding the not coated hexagonal boron nitride powder in surface.The ceramic body prepared is prepared into the ceramic batten of 3mm × 4mm × 30mm through cutting processing-corase grind-fine grinding-grinding-polishing step.Recording its mechanical property parameters is: Vickers' hardness 11.1GPa, fracture toughness property 6.8MPam
1/2, bending strength 599MPa.When joining pair with 45 steel, frictional coefficient is 0.35.
Claims (10)
1. one kind is added the preparation method of the nitride silicon based self-lubrication ceramic cutter material of alumina-coated hexagonal boron nitride composite powder, feed composition volume percent is: micron silicon nitride 57-70%, nano-silicon nitride 5-15%, micrometer silicon carbide titanium 5-15%, aluminum oxide 3.2%, yttrium oxide 4.8%, alumina-coated hexagonal boron nitride 2-15%;
Comprise step as follows:
(1) hexagonal boron nitride powder and the dispersion agent polyoxyethylene glycol of getting particle diameter 3-10 μm are mixed in the hexagonal boron nitride suspension that distilled water is made into 3-8g/L, and dispersion agent addition is the 3-5% of hexagonal boron nitride quality.Add acetic acid-sodium acetate buffer solution that pH value is 4.5, ultrasonic disperse is also stirred and heated to 30 DEG C-40 DEG C, slowly drips Al
3+concentration is the aluminum nitrate solution of 0.1-0.2mol/L, the add-on of described aluminum nitrate solution is according to mol ratio BN: Al=1: 0.5-1 meter, slowly dripping ammoniacal liquor to reacting liquid pH value is again 7.0-7.5, dropwise and keep temperature 30 DEG C-40 DEG C reaction 1.5-2.5h, then still aging, sedimentation and filtration, cleaning, the hexagonal boron nitride composite powder that centrifugal, vacuum-drying obtains Surface coating aluminium hydroxide, through vacuum calcining, the alumina-coated hexagonal boron nitride composite powder of obtained particle diameter 4-12 μm;
(2) in proportion, a micron silicon nitride is taken respectively, nano-silicon nitride, micrometer silicon carbide titanium, with appropriate dehydrated alcohol for dispersion medium, be configured to a micron silicon nitride, micrometer silicon carbide titanium suspension and nano silicon nitride silicon suspension respectively, ultrasonic disperse 15-20min while of well-beaten; Scattered micron silicon nitride, micrometer silicon carbide titanium suspension and nano silicon nitride silicon suspension are mixed, then adds described aluminum oxide, yttrium oxide in proportion, fully stir and ultrasonic disperse 15-20min; Obtain complex phase suspension
(3) above-mentioned complex phase suspension is poured in ball grinder, be filled with argon gas or nitrogen as shielding gas, add ball milling ball, ball milling 36-48h, mixture after ball milling, taking the alumina-coated hexagonal boron nitride composite powder of step (1) in proportion, take dehydrated alcohol as dispersion medium, be made into suspension, ultrasonic disperse 10min; Gained suspension is added in the mixture after ball milling, is filled with argon gas or nitrogen as shielding gas, adds ball milling ball, continue ball milling 8-12h.Then take out ball milling liquid and be placed in loft drier, vacuum-drying 24-36h under 100-120 DEG C of condition; After drying completely, gained mixed powder is crossed 200 mesh sieves, obtain mixed powder, seal for subsequent use;
(4) vacuum hot-pressed sintered technology is adopted, the mixed powder pressing mold sinter molding obtained by step (3).
2. the preparation method adding the nitride silicon based self-lubrication ceramic cutter material of alumina-coated hexagonal boron nitride composite powder as claimed in claim 1, it is characterized in that described feed composition volume percent is micron silicon nitride 62-67%, nano-silicon nitride 10%, micrometer silicon carbide titanium 10%, aluminum oxide 3.2%, yttrium oxide 4.8%, alumina-coated hexagonal boron nitride 5-10%.
3. the as claimed in claim 1 preparation method adding the nitride silicon based self-lubrication ceramic cutter material of alumina-coated hexagonal boron nitride composite powder, is characterized in that the stirring heating described in step (1) is magnetic agitation heating in digital display heat-collecting magnetic stirring device.
4. the preparation method adding the nitride silicon based self-lubrication ceramic cutter material of alumina-coated hexagonal boron nitride composite powder as claimed in claim 1, it is characterized in that described in step (1), pH buffered soln addition is 8-15mL/100mL distilled water, preferably pH buffered soln addition is 10-11mL/100mL distilled water further; Preferred pH pH value of buffer solution is 4.5.
5. the preparation method adding the nitride silicon based self-lubrication ceramic cutter material of alumina-coated hexagonal boron nitride composite powder as claimed in claim 1, it is characterized in that the ammoniacal liquor described in step (1), be with mass percent be the strong aqua distilled water diluting 5-10 of 28% doubly, obtain the ammonia soln that pH value is 6.5-8.5.
6. the preparation method adding the nitride silicon based self-lubrication ceramic cutter material of alumina-coated hexagonal boron nitride composite powder as claimed in claim 1, what it is characterized in that described in step (1) is still aging, be that suspension is carried out standing 10-12 hour, reactant is fully precipitated; Distilled water wash 2-3 time, absolute ethanol washing 2-3 time are used in described washing respectively.
7. the preparation method adding the nitride silicon based self-lubrication ceramic cutter material of alumina-coated hexagonal boron nitride composite powder as claimed in claim 1, it is characterized in that the vacuum calcining described in step (1), be by drying completely the coated hexagonal boron nitride composite powder of aluminium hydroxide be placed in alumina crucible, vacuum calcining in vacuum sintering funace, temperature rise rate is 8-12 DEG C/min, sintering temperature is 1100-1200 DEG C, soaking time is 1.5-2.5h, obtained alumina-coated hexagonal boron nitride composite powder.
8. the preparation method adding the nitride silicon based self-lubrication ceramic cutter material of alumina-coated hexagonal boron nitride composite powder as claimed in claim 1, it is characterized in that the ball milling ball described in step (3) is Wimet (YG8) ball, the addition of ball milling ball is 10 times of each component raw material total mass.
9. the preparation method adding the nitride silicon based self-lubrication ceramic cutter material of alumina-coated hexagonal boron nitride composite powder as claimed in claim 1, it is characterized in that vacuum hot-pressed sintered technology in described step (4), be first load in graphite jig by powder, coldmoulding 15min carries out hot pressed sintering again.
10. the preparation method adding the nitride silicon based self-lubrication ceramic cutter material of alumina-coated hexagonal boron nitride composite powder as claimed in claim 1, it is characterized in that in described step (4), hot pressed sintering parameter is: hot pressed sintering temperature 1650-1700 DEG C, soaking time 45-75min, pressure 25-30MPa, temperature rise rate 10-20 DEG C/min.
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| CN105272269A (en) * | 2015-10-20 | 2016-01-27 | 西安邮电大学 | Preparation method of Si3N4/h-BN nano-composite ceramics |
| CN106904947A (en) * | 2017-02-27 | 2017-06-30 | 齐鲁工业大学 | Add self-lubrication ceramic cutter material of h BN@Ni core shell structure composite granules and preparation method thereof |
| CN107353433A (en) * | 2017-07-20 | 2017-11-17 | 西北工业大学 | Nano-sized magnesium hydroxide/hexagonal nanometer boron nitride composite and preparation method |
| CN107586135A (en) * | 2017-09-26 | 2018-01-16 | 陈凌 | Ceramic composite and its preparation method and application |
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| CN113307630A (en) * | 2021-04-28 | 2021-08-27 | 中国有色桂林矿产地质研究院有限公司 | Superfine composite powder and preparation method thereof |
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| CN106904947A (en) * | 2017-02-27 | 2017-06-30 | 齐鲁工业大学 | Add self-lubrication ceramic cutter material of h BN@Ni core shell structure composite granules and preparation method thereof |
| CN106904947B (en) * | 2017-02-27 | 2019-05-28 | 齐鲁工业大学 | Add the self-lubrication ceramic cutter material and preparation method thereof of h-BN@Ni core-shell structure composite granule |
| CN107353433A (en) * | 2017-07-20 | 2017-11-17 | 西北工业大学 | Nano-sized magnesium hydroxide/hexagonal nanometer boron nitride composite and preparation method |
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| CN111547752B (en) * | 2020-05-11 | 2023-02-24 | 齐鲁工业大学 | Alumina-coated nano flaky hexagonal boron nitride composite powder as well as preparation method and application thereof |
| CN111547752A (en) * | 2020-05-11 | 2020-08-18 | 齐鲁工业大学 | Alumina-coated nano flaky hexagonal boron nitride composite powder and preparation method and application thereof |
| CN111574209A (en) * | 2020-05-20 | 2020-08-25 | 齐鲁工业大学 | Self-lubricating ceramic cutter with self-repairing capability and preparation method, repairing method and application thereof |
| CN111485155A (en) * | 2020-06-09 | 2020-08-04 | 齐鲁工业大学 | (Ti, W) C-based metal ceramic cutting tool material added with alumina coated cubic boron nitride composite powder and preparation method thereof |
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| CN114394596A (en) * | 2021-12-30 | 2022-04-26 | 铜陵日飞创客科技有限公司 | Special long-life bearing for high-power plowing plough |
| CN114394596B (en) * | 2021-12-30 | 2023-08-22 | 铜陵日飞创客科技有限公司 | Special long-life bearing of high-power plough |
| CN116218262A (en) * | 2023-02-15 | 2023-06-06 | 广西大学 | Preparation method of boiler water-cooled wall slag-bonding-preventing nano composite ceramic coating |
| CN116376321A (en) * | 2023-03-30 | 2023-07-04 | 武汉理工大学 | Preparation method and application of aluminum oxide coated hexagonal boron nitride composite powder |
| CN116376321B (en) * | 2023-03-30 | 2024-06-04 | 武汉理工大学 | Preparation method and application of aluminum oxide coated hexagonal boron nitride composite powder |
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