CN106495699A - A kind of SLS technology is combined with PIP technology the method for preparing high-strength high temperature-resistant SiC ceramic guided missile head shell - Google Patents
A kind of SLS technology is combined with PIP technology the method for preparing high-strength high temperature-resistant SiC ceramic guided missile head shell Download PDFInfo
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Abstract
A kind of SLS technology is combined with PIP technology the method for preparing high-strength high temperature-resistant SiC ceramic guided missile head shell.The invention belongs to the 3D printing field of SiC ceramic, more particularly to a kind of SLS technology is combined with PIP technology the method for preparing high-strength high temperature-resistant SiC ceramic guided missile head shell.The invention aims to it is low to solve the problems, such as that existing at present ceramic 3D printing preparation is only limitted to preliminarily forming, low intensity and consistency.Method：First, threedimensional model is built, is then converted into STL formatted files；2nd, STL formatted files are imported 3D printer layered shaping；3rd, SiC powder and binder powder are mixed；4th, print layer by layer；5th, excessive powder is removed；6th, high temperature furnace sintering；7th, infiltration pyrolysis densification, obtains high-strength high temperature-resistant SiC ceramic guided missile head shell.Intensity is 150～200MPa, and porosity is 10～20%, and consistency is high, and intensity is high.
Description
Technical field
The invention belongs to the 3D printing field of SiC ceramic, more particularly to a kind of SLS technology is combined with PIP technology preparation
The method of high-strength high temperature-resistant SiC ceramic guided missile head shell.
Background technology
SiC ceramic has an excellent mechanical property, high bending strength, excellent non-oxidizability, good corrosion resistance, height
Wear-resistant and low coefficient of friction, and mechanical behavior under high temperature (intensity, creep resistance etc.) be in known ceramic material most
Good.Hot pressed sintering, pressureless sintering, the material of HIP sintering, its elevated temperature strength can be maintained to 1600 DEG C, be pottery
The best material of material high temperature intensity.Thus can be described as making the best use of everything with SiC manufacture spacecrafts.
Ceramic forming material method mainly has at present：Extrusion molding, injection moulding, isostatic pressing, flow casting molding etc., this
A little methods are required for mould in preparation process, once design size changes or adjustment will need to redesign and manufacture mould,
And manufacture die cost is higher, the cycle is longer.And limited by the complexity of mould, these techniques are suitable for preparing shape letter
Single product.
With industrial expansion, these traditional techniques can not meet the demand of high-tech product.3D printing is quick
Forming technique is a kind of novel forming technology fast-developing in recent years, and the technology utilization computer software design component passes through
Software hierarchy is discrete and numerical control molding system, using the modes such as laser beam, hot melt nozzle by metal dust, ceramic powders, plastics,
The special materials such as histiocyte are successively piled up bonding, are finally superimposed molding, are produced entity products.The technique with tradition into
Type method is compared, and is had the characteristics that：(1) complex-shaped high-tech product can be prepared；(2) preparation process is without the need for mould,
Save time cycle is short；(3) computer software can be easily passed through and changes design size and shape, greatly shorten new product development
Time；(4) can preparation structure small electronic ceramics product the advantages of.Therefore, rapid shaping technique is subject to widely in recent years
Concern, especially space industry receives much concern.3D printing art mainly has stereolithography technology (SLA), selective laser at present
Sintering (SLS), layer separated growth (LOM), 3 D-printing (3DP) etc., wherein can be applicable to Selective Laser Sintering
Material is more extensive.
However, the 3D printing of existing pottery at present is prepared and is also only limitted to preliminarily forming, the further lifting of its intensity is ground
Study carefully limited, intensity is 5MPa～20MPa, and porosity is 45%～60%, and low intensity, consistency are low, causes ceramic 3D printing to be produced
Product are not applied well.
Content of the invention
The invention aims to solve at present existing pottery 3D printing prepare be only limitted to preliminarily forming, low intensity and
The low problem of consistency, and a kind of SLS technology of offer is combined with PIP technology and prepares high-strength high temperature-resistant SiC ceramic guided missile head
The method of shell.
A kind of SLS technology of the present invention is combined with PIP technology and prepares high-strength high temperature-resistant SiC ceramic guided missile head shell
Method is carried out according to the following steps：
First, the threedimensional model of guided missile head shell is built, threedimensional model is converted to STL formatted files then；
2nd, STL formatted files are imported 3D printer, threedimensional model is layered by the layered shaping software of 3D printer
Process；
3rd, SiC powder and binder powder are added mixer, mixes 8h～24h, obtain the ceramics of uniform particle sizes
End；
4th, the ceramic powders of the uniform particle sizes for obtaining step 3 are added in the barrel of 3D printer, and pave powder,
Then the work box of 3D printer is heated to temperature for 30～70 DEG C, is obtained according to step 2 by the laser head of 3D printer
Individual-layer data print layer by layer from the bottom to top, be obtained ceramic body；Described is 0.05mm～0.2mm per thickness degree；
5th, the work chamber door of 3D printer is opened, ceramic body is placed under room temperature environment 20min～60min, taken out
Excessive powder is removed afterwards；
6th, the ceramic body that removes after excessive powder is put into high temperature furnace sintering, obtains SiC ceramic guided missile head housing department
Part；The sintering furnace sintering temperature is 1000～1600 DEG C, and temperature retention time is 30min～90min；
7th, by high temperature sintering after SiC ceramic guided missile head case member carry out multiple infiltration pyrolysis densification to before comparing
Till rate of body weight gain after single-steeping cracking densification is less than 1%, high-strength high temperature-resistant SiC ceramic guided missile head shell is obtained；Institute
It is that the SiC ceramic guided missile head case member for first obtaining step 6 is put in impregnation liquid to state infiltration pyrolysis densification detailed process
Row dipping, then carries out cured, finally carries out Pintsch process, and Pintsch process temperature is 1000～1400 DEG C, Pintsch process
Time is 30min～90min.
Beneficial effects of the present invention：
The present invention devises the technique that selective laser sintering is combined with PIP methods (infiltration pyrolysis densification), the present invention
Process is simple, material installation low cost, and short preparation period, clout can be reused, and final strength of parts is 150MPa
～200MPa, porosity are 10%～20%, and consistency is high, and intensity is high, and is not limited by ceramic particle species and part shape
System, can prepare various high-strength high temperature-resistant ceramic components, and prepared pottery can be applicable to manufacture outside guided missile head through post processing
Shell.
Description of the drawings
Fig. 1 is that a kind of SLS technology of the present invention is combined with PIP technology and prepares high-strength high temperature-resistant SiC ceramic guided missile head
The flow chart of the method for shell；
Fig. 2 is the structural representation of high-strength high temperature-resistant SiC ceramic guided missile head shell prepared by the present invention.
Specific embodiment
Specific embodiment one：A kind of SLS technology of present embodiment is combined with PIP technology and prepares high-strength high temperature-resistant
The method of SiC ceramic guided missile head shell is carried out according to the following steps：
First, the threedimensional model of guided missile head shell is built, threedimensional model is converted to STL formatted files then；
2nd, STL formatted files are imported 3D printer, threedimensional model is layered by the layered shaping software of 3D printer
Process；
3rd, SiC powder and binder powder are added mixer, mixes 8h～24h, obtain the ceramics of uniform particle sizes
End；
4th, the ceramic powders of the uniform particle sizes for obtaining step 3 are added in the barrel of 3D printer, and pave powder,
Then the work box of 3D printer is heated to temperature for 30～70 DEG C, is obtained according to step 2 by the laser head of 3D printer
Individual-layer data print layer by layer from the bottom to top, be obtained ceramic body；Described is 0.05mm～0.2mm per thickness degree；
5th, the work chamber door of 3D printer is opened, ceramic body is placed under room temperature environment 20min～60min, taken out
Excessive powder is removed afterwards；
6th, the ceramic body that removes after excessive powder is put into high temperature furnace sintering, obtains SiC ceramic guided missile head housing department
Part；The sintering furnace sintering temperature is 1000～1600 DEG C, and temperature retention time is 30min～90min；
7th, by high temperature sintering after SiC ceramic guided missile head case member carry out multiple infiltration pyrolysis densification to before comparing
Till rate of body weight gain after single-steeping cracking densification is less than 1%, high-strength high temperature-resistant SiC ceramic guided missile head shell is obtained；Institute
It is that the SiC ceramic guided missile head case member for first obtaining step 6 is put in impregnation liquid to state infiltration pyrolysis densification detailed process
Row dipping, then carries out cured, finally carries out Pintsch process, and Pintsch process temperature is 1000～1400 DEG C, Pintsch process
Time is 30min～90min.
Specific embodiment two：Present embodiment from unlike specific embodiment one：UG softwares used in step one
Threedimensional model is converted to STL formatted files.Other steps and parameter are identical with specific embodiment one.
Specific embodiment three：Present embodiment from unlike specific embodiment one or two：3D described in step 2
Printer is selective laser sintering printer.Other steps and parameter are identical with specific embodiment one or two.
Specific embodiment four：Unlike one of present embodiment and specific embodiment one to three：Institute in step 3
The weight/mass percentage composition for stating SiC powder in ceramic powders is 80%～95%, balance of binder powder.Other steps and parameter
Identical with one of specific embodiment one to three.
Specific embodiment five：Unlike one of present embodiment and specific embodiment one to four：Institute in step 3
The weight/mass percentage composition for stating SiC powder in ceramic powders is 90%, balance of binder powder.Other steps and parameter with concrete
One of embodiment one to four is identical.
Specific embodiment six：Unlike one of present embodiment and specific embodiment one to five：Institute in step 3
The mean diameter for stating ceramic powders is 1 μm～120 μm.One of other steps and parameter and specific embodiment one to five are identical.
Specific embodiment seven：Unlike one of present embodiment and specific embodiment one to six：Institute in step 3
Binder powder is stated for epoxy powder, dextrin powder, ammonium polyacrylate powder or polyethylene glycol powder.Other steps and ginseng
Number is identical with one of specific embodiment one to six.
Specific embodiment eight：Unlike one of present embodiment and specific embodiment one to seven：Will in step 4
The ceramic powders of the uniform particle sizes that step 3 is obtained are added in the barrel of 3D printer, and pave powder, then by 3D printing
The work box of machine is heated to temperature for 55 DEG C.One of other steps and parameter and specific embodiment one to seven are identical.
Specific embodiment nine：Unlike one of present embodiment and specific embodiment one to eight：Institute in step 6
Sintering furnace sintering temperature is stated for 1400 DEG C, temperature retention time is 60min.Other steps and parameter and specific embodiment one to eight it
One is identical.
Specific embodiment ten：Unlike one of present embodiment and specific embodiment one to nine：Institute in step 7
Impregnation liquid is stated for Polycarbosilane/divinylbenzene precursor solution, poly- carbon silicon in Polycarbosilane/divinylbenzene precursor solution
Alkane and the mass ratio 1 of divinylbenzene:4.One of other steps and parameter and specific embodiment one to nine are identical.
Specific embodiment 11：Unlike one of present embodiment and specific embodiment one to ten：In step 7
The dipping process is specially：The SiC ceramic guided missile head case member for first obtaining step 6 is put in impregnation liquid, is then proceeded to
In dipping stove, evacuation 30min under conditions of temperature is for 65 DEG C, then pressurize under conditions of temperature is for 65 DEG C 30min, pressure
Power is 0.2MPa.One of other steps and parameter and specific embodiment one to ten are identical.
Specific embodiment 12：Unlike one of present embodiment and specific embodiment one to ten one：Step 7
Described in solidify detailed process be：It is placed in Constant Temp. Oven, first solidification 3h under conditions of temperature is for 120 DEG C, then
Temperature is solidification 3h under conditions of 150 DEG C.One of other steps and parameter and specific embodiment one to ten one are identical.
Specific embodiment 13：Unlike one of present embodiment and specific embodiment one to ten two：Step 7
Described in Pintsch process temperature be 1200 DEG C, the Pintsch process time be 60min.Other steps and parameter and specific embodiment one
Identical to one of 12.
The effect of the present invention is verified with following experiment
A kind of test one, SLS technology of this test is combined with PIP technology and prepares high-strength high temperature-resistant SiC ceramic guided missile
The method of head shell is carried out according to the following steps：
First, the threedimensional model of guided missile head shell is built, threedimensional model is converted to STL formatted files then；
2nd, STL formatted files are imported 3D printer, threedimensional model is layered by the layered shaping software of 3D printer
Process；
3rd, SiC powder and binder powder are added mixer, mixes 8h～24h, obtain the ceramics of uniform particle sizes
End；
4th, the ceramic powders of the uniform particle sizes for obtaining step 3 are added in the barrel of 3D printer, and pave powder,
Then the work box of 3D printer is heated to temperature for 55 DEG C, by the laser head of 3D printer according to dividing that step 2 is obtained
Layer data is printed from the bottom to top layer by layer, and ceramic body is obtained；Described is 0.1mm per thickness degree；
5th, the work chamber door of 3D printer is opened, ceramic body is placed 60min under room temperature environment, removed after taking-up
Excessive powder；
6th, the ceramic body that removes after excessive powder is put into high temperature furnace sintering, obtains SiC ceramic guided missile head housing department
Part；The sintering furnace sintering temperature is 1400 DEG C, and temperature retention time is 60min；
7th, by high temperature sintering after SiC ceramic guided missile head case member carry out multiple infiltration pyrolysis densification to before comparing
Till rate of body weight gain after single-steeping cracking densification is less than 1%, high-strength high temperature-resistant SiC ceramic guided missile head shell is obtained；Institute
It is that the SiC ceramic guided missile head case member for first obtaining step 6 is put in impregnation liquid to state infiltration pyrolysis densification detailed process
Row dipping, then carries out cured, finally carries out Pintsch process, and Pintsch process temperature is 1200 DEG C, and the Pintsch process time is
60min.
Used in step one, threedimensional model is converted to STL formatted files by UG softwares.
3D printer described in step 2 is selective laser sintering printer.
Described in step 3, in ceramic powders, the weight/mass percentage composition of SiC powder is 90%, balance of binder powder.
The mean diameter of ceramic powders described in step 3 is 70 μm.
Binder powder described in step 3 is epoxy powder.
Impregnation liquid described in step 7 be Polycarbosilane/divinylbenzene precursor solution, Polycarbosilane/divinylbenzene
The mass ratio 1 of Polycarbosilane and divinylbenzene in precursor solution:4.
Described in step 7, dipping process is specially：The SiC ceramic guided missile head case member for first obtaining step 6 is put into
In impregnation liquid, then proceed in dipping stove, be evacuation 30min under conditions of 65 DEG C in temperature, be then 65 DEG C in temperature
Under the conditions of pressurize 30min, pressure is 0.2MPa.
Solidifying detailed process described in step 7 is：It is placed in Constant Temp. Oven, first in the condition that temperature is 120 DEG C
Lower solidification 3h, then solidify 3h under conditions of temperature is for 150 DEG C.
The high-strength high temperature-resistant SiC ceramic guided missile head shell that this test is obtained after testing, its intensity are 185MPa, porosity
For 20%.
Claims (10)
1. a kind of SLS technology is combined with PIP technology the method for preparing high-strength high temperature-resistant SiC ceramic guided missile head shell, and which is special
Levy and be that the method is carried out according to the following steps：
First, the threedimensional model of guided missile head shell is built, threedimensional model is converted to STL formatted files then；
2nd, by STL formatted files import 3D printer, by the layered shaping software of 3D printer to threedimensional model layering at
Reason；
3rd, SiC powder and binder powder are added mixer, mixes 8h～24h, obtain the ceramic powders of uniform particle sizes；
4th, the ceramic powders of the uniform particle sizes for obtaining step 3 are added in the barrel of 3D printer, and pave powder, then
The work box of 3D printer is heated to temperature for 30～70 DEG C, by the laser head of 3D printer according to dividing that step 2 is obtained
Layer data is printed from the bottom to top layer by layer, and ceramic body is obtained；Described is 0.05mm～0.2mm per thickness degree；
5th, the work chamber door of 3D printer is opened, ceramic body is placed 20min～60min under room temperature environment, clear after taking-up
Remove excessive powder；
6th, the ceramic body that removes after excessive powder is put into high temperature furnace sintering, obtains SiC ceramic guided missile head case member；Institute
Sintering furnace sintering temperature is stated for 1000～1600 DEG C, temperature retention time is 30min～90min；
7th, by high temperature sintering after SiC ceramic guided missile head case member carry out multiple infiltration pyrolysis densification to before comparing once
Till rate of body weight gain after infiltration pyrolysis densification is less than 1%, high-strength high temperature-resistant SiC ceramic guided missile head shell is obtained；The leaching
Stain cracking densification detailed process is that the SiC ceramic guided missile head case member for first obtaining step 6 is put in impregnation liquid and is soaked
Stain, then carries out cured, finally carries out Pintsch process, and Pintsch process temperature is 1000～1400 DEG C, the Pintsch process time
For 30min～90min.
2. a kind of SLS technology according to claim 1 is combined with PIP technology and prepares high-strength high temperature-resistant SiC ceramic and lead
The method of bullet shell, it is characterised in that threedimensional model is converted to STL formatted files by UG softwares used in step one.
3. a kind of SLS technology according to claim 1 is combined with PIP technology and prepares high-strength high temperature-resistant SiC ceramic and lead
The method of bullet shell, it is characterised in that 3D printer described in step 2 is selective laser sintering printer.
4. a kind of SLS technology according to claim 1 is combined with PIP technology and prepares high-strength high temperature-resistant SiC ceramic and lead
The method of bullet shell, it is characterised in that described in step 3 in ceramic powders SiC powder weight/mass percentage composition be 80%～
95%, balance of binder powder.
5. a kind of SLS technology according to claim 1 is combined with PIP technology and prepares high-strength high temperature-resistant SiC ceramic and lead
The method of bullet shell, it is characterised in that the mean diameter of ceramic powders described in step 3 is 1 μm～120 μm.
6. a kind of SLS technology according to claim 1 is combined with PIP technology and prepares high-strength high temperature-resistant SiC ceramic and lead
The method of bullet shell, it is characterised in that binder powder described in step 3 is epoxy powder, dextrin powder, polypropylene
Sour ammonium powder or polyethylene glycol powder.
7. a kind of SLS technology according to claim 1 is combined with PIP technology and prepares high-strength high temperature-resistant SiC ceramic and lead
The method of bullet shell, it is characterised in that the ceramic powders of the uniform particle sizes in step 4 obtaining step 3 are added to 3D printing
In the barrel of machine, and powder is paved, the work box of 3D printer is heated to temperature for 55 DEG C then.
8. a kind of SLS technology according to claim 1 is combined with PIP technology and prepares high-strength high temperature-resistant SiC ceramic and lead
The method of bullet shell, it is characterised in that impregnation liquid described in step 7 is Polycarbosilane/divinylbenzene precursor solution, gathers
The mass ratio 1 of Polycarbosilane and divinylbenzene in carbon silane/divinylbenzene precursor solution:4.
9. a kind of SLS technology according to claim 1 is combined with PIP technology and prepares high-strength high temperature-resistant SiC ceramic and lead
The method of bullet shell, it is characterised in that dipping process is specially described in step 7：First the SiC ceramic that step 6 is obtained is led
Bullet case member is put in impregnation liquid, is then proceeded in dipping stove, evacuation 30min under conditions of temperature is for 65 DEG C, so
Pressurize under conditions of temperature is for 65 DEG C 30min afterwards, and pressure is 0.2MPa.
10. a kind of SLS technology according to claim 1 is combined with PIP technology and prepares high-strength high temperature-resistant SiC ceramic and lead
The method of bullet shell, it is characterised in that solidifying detailed process described in step 7 is：It is placed in Constant Temp. Oven, first exists
Temperature is solidification 3h under conditions of 120 DEG C, then under conditions of temperature is for 150 DEG C solidifies 3h.
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| CN107253861A (en) * | 2017-07-05 | 2017-10-17 | 哈尔滨理工大学 | A kind of method that SLS/CVI prepares high-strength high temperature-resistant SiC ceramic engine blade wheel |
| CN107602130A (en) * | 2017-10-17 | 2018-01-19 | 哈尔滨理工大学 | The method that porous SiC ceramics are prepared based on 3D forming techniques |
| CN108264353A (en) * | 2018-01-25 | 2018-07-10 | 哈尔滨理工大学 | A kind of SiCwThe preparation method of/SiC/SiC ceramic matric composites |
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| CN109280395A (en) * | 2017-07-19 | 2019-01-29 | 北京恒创增材制造技术研究院有限公司 | A kind of product and preparation method thereof of photocurable quick shaping process preparation |
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| CN112851354A (en) * | 2021-01-29 | 2021-05-28 | 汕头大学 | Porous structure ceramic and preparation method thereof |
| CN116444275A (en) * | 2023-04-26 | 2023-07-18 | 哈尔滨理工大学 | Method for preparing low-porosity SiC ceramic matrix composite by combining SLS and PIP |
| CN116675538A (en) * | 2023-05-30 | 2023-09-01 | 中国科学院上海硅酸盐研究所 | Method for preparing SiC ceramic by combining selective laser 3D printing/precursor dipping pyrolysis/liquid phase sintering |
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| CN116675538A (en) * | 2023-05-30 | 2023-09-01 | 中国科学院上海硅酸盐研究所 | Method for preparing SiC ceramic by combining selective laser 3D printing/precursor dipping pyrolysis/liquid phase sintering |
| CN116675538B (en) * | 2023-05-30 | 2023-12-22 | 中国科学院上海硅酸盐研究所 | Method for preparing SiC ceramic by combining selective laser 3D printing/precursor dipping pyrolysis/liquid phase sintering |
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