Labyrinth silicon carbide ceramic part manufacture method based on laser 3D printing technique
Technical field
The invention belongs to ceramic materials preparation technology field, be specifically related to a kind of complicated knot based on laser 3D printing technique
Structure silicon carbide ceramic part manufacture method.
Background technology
Thyrite is a kind of ceramic material with premium properties such as high temperature resistant, wear-resistant, acid and alkali-resistances, extensively
It is applied to the fields such as Aero-Space, electronic manufacture, vehicle naval vessel.But, due to the feature that carbofrax material hardness is high, fragility is big
Cause the part forming of labyrinth, process extremely difficult, traditional process and typically need to complete zero by complicated mould
Part shapes.In the information age of today, the update speed of product is very fast, and the exploitation manufacture of complicated die needs to put into
More time and cost, it is clear that this is easy to disconnect with market.
Laser 3D printing technique is a kind of method of forming materials based on discrete/accumulation principle, and this technology uses CAD software
Draw 3D solid in a computer, the discrete and numerical control molding system by software hierarchy, utilize laser beam by metal dust, pottery
Porcelain powder, plastic or other material are successively piled up, and produce entity products.Utilize laser 3D printing technique to be molded carborundum pottery
Porcelain powder has the advantage that (1) is not necessarily to mould, makes production process more integrated, shortens the manufacturing cycle, improves production
Efficiency;(2) product of labyrinth can be molded;(3) formed body geometry and size can be according to actual needs by meters
Calculation machine software modification, it is not necessary to wait mould design and manufacture, be greatly shortened the development time of new product.
At present, typical laser 3D printing technique include selective laser sintering (Selective Laser Sintering,
And selective laser fusing (Selective Laser Melting, SLM) etc. SLS).The sintering temperature of thyrite is high,
If using the shaping of SLM direct sintering, owing to rapid heating and cooling effect easilys lead to product, crackle occurs.If using SLS technology to become
Type silicon carbide ceramic part, needs first to prepare resin adhesive/silicon carbide ceramics composite powder material, then puts SLS equipment into
Carry out laser sintering and moulding and obtain ceramic body, then pyrolysis processing is carried out to base substrate remove resinoid bond.At pyrolytic process
Many holes can be produced in middle base substrate, in order to obtain the silicon carbide products of densification, finally the base substrate after pyrolysis would generally be carried out
Siliconising reaction-sintered.During additionally, above-mentioned SLS technological forming silicon carbide ceramic part there is problems in that (1) whole technological process
Between long;(2) pyrolysis removes in adhesive process, and the hole of generation can cause the density of base substrate, intensity to decline, and fragility increases, sternly
The situation of weight can make base substrate defeated and dispersed;(3) during siliconising, siliconising amount is wayward, easily produces silicon enrichment so that material
Become fragile, creep-resistant property reduces, and in base substrate, siliconising path easily blocks, and causes blank strength uneven, easily produces
The critical defects such as crackle, reduce yield rate.
Content of the invention
It is an object of the invention to solve problems present in existing silicon carbide ceramic part manufacture process, provide one
Plant the labyrinth silicon carbide ceramic part manufacture method based on laser 3D printing technique.The method is simple to operate easy to spread to be made
With, it is not necessary to follow-up siliconising step can be prepared by intensity silicon carbide ceramic part higher, baroque.Technical scheme
As follows:
A kind of labyrinth silicon carbide ceramic part manufacture method based on laser 3D printing technique, comprises the following steps:
A () weighs silicon carbide ceramics powder, binding agent, silicon source material, carbon source material in required ratio, put above-mentioned raw materials
Enter in ball grinder and add enough organic solvents, batch mixing uniformly afterwards heating make solvent volatilize to obtain composite silicon carbide ceramic powder.
B () is placed in composite silicon carbide ceramic powder in laser 3D printer and preheats, according to the model layer layer stack of design
Long-pending formed ceramic parts just base.
C () is placed in ceramic part just base in protective atmosphere and carries out pyrolysis processing.
D the ceramic part after () pyrolysis is sintered according to certain calcining system, obtain the carborundum pottery of labyrinth
Porcelain part.
In such scheme, one in phenolic resin, epoxy resin, stearic acid, paraffin for the binding agent, silicon source material selects
One in silica flour, silica flour, one in carbon black, graphite powder, starch for the carbon source material, described organic solvent is first
One in alcohol, ethanol, acetone.
In such scheme, the mass percent that silicon carbide powder accounts for solid material is 60-85%, and binding agent accounts for solid material
Mass percent be 10-30%, the mass percent that silicon source material accounts for solid material is 1-20%, balance of carbon source material.
In step (a), mixing time is 6-12h, and compound is first placed in after mixing heating evaporation in magnetic stirring apparatus
Go out partial solvent, when remaining a small amount of liquid flux, compound is taken out and be placed in air heating, will after solvent volatilizees completely
Compound put in vacuum drying chamber be dried 24 hours, until its be cooled to after room temperature through grind, sieve to obtain composite silicon carbide ceramic
Powder.
In step (b), composite silicon carbide ceramic powder is preheated to 50-90 DEG C in laser 3D printer, laser 3D printer
The laser instrument using is carbon dioxide laser, and laser power scope is 0-200W.
In step (c), ceramic part just base is pyrolyzed in argon gas atmosphere in such a way: from room temperature with 3-5 DEG C/
The heating rate of min is warmed up to 110 DEG C and keeps 30-60min, and then the heating rate with 5 DEG C/min is warmed up to 830 DEG C and protects
Temperature 2-3h, finally the rate of temperature fall with 1-2 DEG C/min is cooled to room temperature.
In step (d), the ceramic part vacuum-sintering process after pyrolysis is: heat up from room temperature with the heating rate of 5 DEG C/min
To 2200 DEG C and be incubated 2-3h, then the rate of temperature fall with 1-2 DEG C/min is cooled to room temperature.
Compared to Conventional silicon carbide pottery parts with complex structures forming method, the inventive method has the advantages that
(1) using solvent precipitation to carry out batch mixing, after being dried, binding agent will be coated on silicon carbide ceramics powder, silicon source material, carbon source material
On material, covered effect is good, it is possible to reduce the addition of binding agent thus the number that reduces the retraction volume in sintering process and hole
Amount, improves the intensity of base substrate;(2) stage is printed at laser 3D, owing to using superpower laser, portion of binder directly quilt
Pyrolysis, and carbon source material and silicon source material can occur the hole that pre-reaction sintering stays after forming the pyrolysis of carborundum filling adhesive
Gap, improves green density, makes the intensity of base substrate be guaranteed, decreases the possibility cracking;(3) technological process letter
Single, raw material add silicon source and carbon source, it is not necessary to the high carbonization of consistency can be obtained by operations such as follow-up siliconisings again
Silicon ceramic part, shortens the cycle manufacturing labyrinth silicon carbide ceramic part, reduces cost;It is (4) simple to operate, it is easy to
Promote the use of.
Brief description
Fig. 1 is the inventive method process chart;
Fig. 2 is composite ceramic powder shaping and densified schematic diagram in the inventive method.
Detailed description of the invention
For making those of ordinary skill in the art fully understand technical scheme and beneficial effect, below in conjunction with specifically
Embodiment and accompanying drawing absolutely prove further.
What the present invention provided manufactures the technological process of labyrinth silicon carbide ceramic part such as based on laser 3D printing technique
Shown in Fig. 1, initially with solvent precipitation, silicon carbide ceramics powder, binding agent, silicon source material, carbon source material are fabricated to be combined
Ceramic powders is standby.Recycling 3D sculpting software (such as Catia, UG, Pro/E) design complex configurations ceramic part is simultaneously built
Mould, the threedimensional model completing moulding is output as STL formatted file, is sent to this stl file in laser 3D printing, and use is cut
Piece delamination software carries out layered shaping to STL, then imports data to print in fabrication schedule.Laser 3D printer uses
Laser instrument be carbon dioxide laser, its laser power scope is 0-200W, sets its parameter as follows: lift height 0.05-
0.2mm, filling speed 1800-2500mm/s, laser scanning spacing 0.08-0.3mm, laser scanning power 0-200W, laser wheel
Wide power 5-50W.The pottery printing just base sinters available final products one labyrinth carborundum after pyrolysis processing
Ceramic part.
In print procedure, composite ceramic powder shaping and densified principle are as shown in Figure 2.Prepared by solvent precipitation
In composite powder, binding agent be coated to carborundum, carbon source material, on silicon source material, through laser 3D printing-forming, binding agent
Melt and be bonded together, and part carbon source material sinters with silicon source material generation pre-reaction, in conjunction with formation SiC phase.Pyrolysis
After, binding agent organic cracking, remaining product is the carbon skeleton that carbon carbon connects.Finally, material carries out high temperature sintering, carbon source material
Material reacts generation SiC further with silicon source material, meanwhile, base substance in vivo by different diffusion path to intergranular
Space is filled, and subsequently, tiny particle gradually forms crystal boundary, and constantly expands grain boundary area, makes base substrate gradually fine and close.
Embodiment 1
Weigh each corresponding raw material for standby according to the following ratio: 150 grams of silicon carbide ceramics powder, 50 grams of phenolic resin, silica flour
10 grams, graphite powder 10 grams.
Silicon carbide ceramics powder, phenolic resin, silica flour, graphite powder are put in ball grinder, pour enough acetone solvents into,
Then batch mixing 8 hours on ball mill.In order to enable solvent to vapor away quickly, first mixed mixed liquor is placed in magnetic force
Heating in agitator makes solvent volatilize, and when also remaining a small amount of liquid flux, is drawn off being placed in air heating continuation volatilization molten
Agent, when after solvent volatilizees completely, compound is put in vacuum drying chamber be dried 24 little when, ground after being cooled to room temperature
Sieve, obtain composite silicon carbide ceramic dusty material.
Put into above-mentioned composite silicon carbide ceramic powder in laser 3D printer and be preheating to 90 DEG C.Set laser
After the parameter of 3D printer, print ceramic part just base under program.
Putting into ceramic part just base and carrying out pyrolysis processing in argon atmosphere, pyrolysis processing process is as follows: first from
Room temperature is warmed up to 110 DEG C with the heating rate of 3-5 DEG C/min and keeps 30-60min, then the heating rate liter with 5 DEG C/min
Temperature is to 830 DEG C and is incubated 2-3h, and finally the rate of temperature fall with 1-2 DEG C/min is cooled to room temperature
Finally sintering the ceramic part after pyrolysis in vacuum sintering furnace, sintering process is: from room temperature with 5 DEG C/min
Heating rate is warming up to 2200 DEG C and is incubated 2-3h, and then the rate of temperature fall with 1-2 DEG C/min is cooled to room temperature.Sintering complete with
After obtain the labyrinth silicon carbide ceramic part with higher-strength and toughness.
Embodiment 2
Weigh each corresponding raw material for standby according to the following ratio: 120 grams of silicon carbide ceramics powder, 60 grams of phenolic resin, silica flour 10
Gram, starch 10 grams.
Silicon carbide ceramics powder, phenolic resin, silica flour, starch are put in ball grinder, pours enough acetone solvents into, then
Batch mixing 8 hours on ball mill.Being placed in mixed mixed liquor in magnetic stirring apparatus heating makes solvent volatilize, and treats also to remain on a small quantity
It is drawn off being placed in air heating during liquid flux and continues solvent flashing, after solvent volatilizees completely, compound is put into vacuum
Drying box is dried 24 hours, is ground after being cooled to room temperature and sieve, obtain composite silicon carbide ceramic dusty material.
Put into above-mentioned composite silicon carbide ceramic powder in laser 3D printer and be preheating to 90 DEG C.Set laser
After the parameter of 3D printer, print ceramic part just base under program.
Ceramic part just base is put into the mode according to embodiment 1 in argon atmosphere and carries out pyrolysis processing.
Finally the ceramic part after pyrolysis is sintered according to the calcining system of embodiment 1 in vacuum sintering furnace,
To the labyrinth silicon carbide ceramic part with higher-strength and toughness.
Embodiment 3
Weigh each corresponding raw material for standby according to the following ratio: 120 grams of silicon carbide ceramics powder, epoxy resin 60 grams, silica flour 10
Gram, carbon powder 10 grams.
Silicon carbide ceramics powder, epoxy resin, silica flour, carbon powder are put in ball grinder, pours enough alcohol solvents into, so
After on ball mill batch mixing 9 hours.Being placed in mixed mixed liquor in magnetic stirring apparatus heating makes solvent volatilize, and treats also to remain less
It is drawn off being placed in air heating during quantity of fluid solvent and continues solvent flashing, after solvent volatilizees completely, compound is put into very
Empty drying box is dried 24 hours, is ground after being cooled to room temperature and sieve, obtain composite silicon carbide ceramic dusty material.
Put into above-mentioned composite silicon carbide ceramic powder in laser 3D printer and be preheating to 55 DEG C.Set laser
After the parameter of 3D printer, print ceramic part just base under program.
Ceramic part just base is put into the mode according to embodiment 1 in argon atmosphere and carries out pyrolysis processing.
Finally the ceramic part after pyrolysis is sintered according to the calcining system of embodiment 1 in vacuum sintering furnace,
To the labyrinth silicon carbide ceramic part with higher-strength and toughness.
The raw material of embodiment 4-6 amounts to 100g, and the percetage by weight of each raw material sees following table.Except parameters described below, condition
Outside changing, other techniques and parameter are same as in Example 1, and details see table.
Table 1 embodiment 4-6 contrasts table
The present invention prepares the process of labyrinth ceramic part based on laser 3D printing technique, it is thus achieved that have certain
The labyrinth silicon carbide ceramic part of intensity and toughness.This invention with the addition of silicon source, carbon source material in the middle of powder, at laser
When 3D prints, there is pre-sintering reaction in part silicon source carbon source material, overcomes conventional laser 3D printing technique shaping carborundum pottery
After technological process length that porcelain exists, pyrolysis, blank strength is low, siliconising process easily occurs bad reaction to cause danger to staff
Etc. defect.The technological process of the present invention is simple, can reduce cost, has excellent very greatly on the complicated silicon carbide ceramic part of making
Gesture.
The above, the only present invention preferably detailed description of the invention, but the scope of protection of the invention is not limited thereto,
Any those familiar with the art in the technical scope that the invention discloses, the change that can readily occur in or replacement,
All should cover within protection scope of the present invention.