CN108002842A - A kind of preparation method of complicated shape nitride porous silicon member - Google Patents
A kind of preparation method of complicated shape nitride porous silicon member Download PDFInfo
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Abstract
The invention belongs to material to be molded correlative technology field, it discloses a kind of preparation method of complicated shape nitride porous silicon member, metal laser selective melting technique is combined by this method with the reaction sintering technology of silicon nitride, and to prepare large scale, complicated shape nitride porous silicon parts provide new thinking；Specifically include following steps：(1) metallic silicon power of offer predetermined quality number and oxide sintering aid are as raw material；(2) use selective laser melting process to the raw material carry out microcell partially sinter with it is preforming go out porous silicon base substrate；(3) reaction-sintered is carried out to the porous silicon base substrate, complicated shape nitride porous silicon member is obtained by nitrogenizing.The preparation method easily realizes nitride porous silicon member control shape control, can improve manufacture efficiency, and flexibility is higher, and without high polymer binder.
Description
Technical field
The invention belongs to material to be molded correlative technology field, more particularly, to a kind of complicated shape nitride porous silicon member
Preparation method.
Background technology
For a long time, the preparation of complicated shape porous silicon nitride ceramic part is always to restrict porous silicon nitride ceramic engineering
One of problem of application, for this various countries researchers have developed such as gel injection-moulding, injection forming, extrusion molding, directly solidification
The moulding process of a variety of silicon nitride ceramics complicated shape parts such as injection molding.Although these methods can prepare complicated shape part, equal
Manufacture dependent on mould.Since the mold body manufacturing cycle is long, of high cost so that the manufacture of complicated shape nitride porous silicon member
Cycle and cost are also elevated, particularly small lot, large complicated profiles prepare it is especially true.Increasing material manufacturing skill in recent years
The development of art so that the preparation of complicated shape porous silicon nitride ceramic part can break away from the dependence to mould, realize complicated shape
The mould-free forming of part.
Increases material manufacturing technology is based on discrete-accumulation principle, and raw material is overlapped shaping by point-by-point, by-line or by face
Go out complicated shape part, be one of most promising technical method for solving the problems, such as ceramic complicated shape part difficult forming.Silicon nitride
The common increases material manufacturing technology of ceramics includes selective laser sintering technology (SLS), layer separated growth technology (LOM), photocuring
Technology (SLA) and fusion sediment moulding (FDM) etc., the more ceramic increases material manufacturing technology of current application include indirect laser
The technologies such as constituency sintering technology (indirect SLS), fusion sediment moulding (FDM) and photocuring technology (SLA).But these skills
Art often directly using silicon nitride ceramics powder as raw material, and add polymeric adhesive with realize complicated shape part precast body into
Type, then by high-temperature post-treatment to obtain silicon nitride complicated shape part.To improve the intensity of increasing material manufacturing molding blank, cause
The high molecular content applied during increasing material manufacturing is often higher.This not only needs to increase in subsequent processing to high molecular
Skimming processes, photosensitive resin may turn due to cracking endless congruent reason particularly in the preparation process of large-size ceramic component
It is changed into carbon residue, influences product properties stability.
The content of the invention
For the disadvantages described above or Improvement requirement of the prior art, the present invention provides a kind of complicated shape nitride porous silicon member
Preparation method, its preparation characteristic based on existing complicated shape nitride porous silicon member, studies and devises and is a kind of without using appointing
The preparation method of the complicated shape nitride porous silicon member of what high polymer binder.The preparation method uses metallic silicon and oxide
Sintering aid is raw material, carries out part fusing to material powder using precinct laser fusion technique and sinters, is configured to prefabricated
Body, then porous metals silicon precast body is changed into by nitride porous silicon materials by the method that reaction-sintered nitrogenizes, due in material
Without using any high polymer binder, and the bonding that the bonding of precast body is melted based on metallic particles, thus the intensity of precast body compared with
It is high and influenced without any carbon residue, it is suitable for the preparation of large complicated shape porous silicon nitride part.
To achieve the above object, the present invention provides a kind of preparation method of complicated shape nitride porous silicon member, this method
Comprise the following steps：
(1) metallic silicon power of offer predetermined quality number and oxide sintering aid are as raw material；
(2) use increasing material manufacturing technique to partially sinter the raw material with it is preforming go out porous silicon base substrate；
(3) reaction-sintered is carried out to the porous silicon base substrate, is nitrogenized to obtain complicated shape nitride porous silicon member.
Further, the mass fraction of the metallic silicon power is 80 parts~95 parts, the quality of the oxide sintering aid
Number is 5 parts~20 parts.
Further, the metallic silicon power is the spherical silicon powder that average grain diameter is 1 μm~30 μm, the weight of its impurity contained
Measure percentage and be less than 1%.
Further, the oxide sintering aid is iron oxide, ferrous oxide, yittrium oxide, lanthana, aluminium oxide, oxygen
Change the one or more in zirconium and magnesia.
Further, the particle diameter of the oxide sintering aid is 0.01 μm~10 μm, the weight hundred of its impurity contained
Divide than being less than 0.5%.
Further, the step of mechanical ball mill is carried out to the raw material, ball are further included before the raw material is sintered
Rotating speed during mill is 100 turns~400 turns/min, and the ball milling mixing time is more than 2h.
Further, the increasing material manufacturing technique is selective laser melting process.
Further, the mould using the selective laser melting process according to complicated shape nitride porous silicon member to be formed
Type information successively sinters the raw material, and laser sintered power is 20W~200W, laser scan rate for 2mm/s~
7000mm/s, lift height are 0.05mm~0.2mm.
Further, the porous silicon blank is put into nitrogen sintering furnace, is passed through flowing nitrogen and carries out reaction-sintered, with
Obtain complicated shape nitride porous silicon member.
Further, the heating rate of reaction-sintered is 5 DEG C~15 DEG C/min, and nitrogen pressure is not less than 0.1MPa, and instead
When should sinter 2h is kept the temperature at 1100 DEG C, 1200 DEG C, 1300 DEG C and 1450 DEG C respectively.
In general, by the contemplated above technical scheme of the present invention compared with prior art, it is provided by the invention multiple
The preparation method of miscellaneous shape nitride porous silicon member mainly has the advantages that：
1. the preparation method, as raw material, is bonded directly using metallic silicon and oxide sintering aid without macromolecule
Agent, avoids the problem that high polymer binder introduces carbon residue in large-size components preparation process；
2. carrying out successively fusing to raw material using selective laser melting process to sinter, raw material is pre-formed as porous silicon base
Part, solves during traditional handicraft to porous silicon nitride ceramic to be difficult to prepare complicated shape part dependent on mould molding and asks
Topic, improves manufacture efficiency and control shape ability, flexibility are preferable；
3. due to the bonding melted without using the bonding of any high polymer binder, porous silicon blank based on metallic particles,
Its intensity is higher, without carrying out ungrease treatment, shortens technological process and process cycle prepared by complicated shape nitridation silicon member, fits
It is suitable for the preparation of the porous silicon nitride parts of large complicated shape；
4. the preparation method technique is simple, easy to implement, be conducive to promote and apply.
Brief description of the drawings
Fig. 1 is the flow signal of the preparation method for the complicated shape nitride porous silicon member that better embodiment of the present invention provides
Figure.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to the accompanying drawings and embodiments, it is right
The present invention is further elaborated.It should be appreciated that specific embodiment described herein is only to explain the present invention, not
For limiting the present invention.As long as in addition, technical characteristic involved in each embodiment of invention described below that
Not forming conflict between this can be mutually combined.
Referring to Fig. 1, the preparation method for the complicated shape nitride porous silicon member that better embodiment of the present invention provides, described
Preparation method uses metallic silicon and oxide sintering aid as raw material, using precinct laser fusion technique to material powder carry out portion
Divide fusing sintering, be configured to precast body, then be changed into porous metals silicon precast body by the method that reaction-sintered nitrogenizes
Nitride porous silicon materials, since, without using any high polymer binder, and the bonding of precast body is based on metallic particles portion in material
The bonding for dividing fusing to be formed, therefore the intensity of precast body is higher and is influenced without any carbon residue, is suitable for the porous nitrogen of large complicated shape
The preparation of SiClx part.
The preparation method of the complicated shape nitride porous silicon member mainly includes the following steps that：
Step 1, there is provided the metallic silicon power and oxide sintering aid of predetermined quality number are as raw material.Specifically, it is described
The mass fraction of metallic silicon power is 80 parts~95 parts, and the mass fraction of the oxide sintering aid is 5 parts~20 parts, i.e., described
The mass ratio of metallic silicon power and the oxide sintering aid is (80~95)：(5~20).
In present embodiment, the metallic silicon power is the spherical silicon powder that average grain diameter is 1 μm~30 μm, its impurity contained
Percentage by weight be less than 1%；The oxide sintering aid for iron oxide, ferrous oxide, yittrium oxide, lanthana, aluminium oxide,
One or more in zirconium oxide and magnesia, the particle diameter of the oxide sintering aid is 0.01 μm~10 μm, it contains
Impurity percentage by weight be less than 0.5%.
Step 2, use increasing material manufacturing technique to partially sinter the raw material with it is preforming go out porous silicon base substrate.It is excellent
Selection of land is that the increasing material manufacturing technique is selective laser melting process.
Further included before the raw material is sintered to the raw material carry out mechanical ball mill with obtain mixed-powder or
The raw material is granulated as 30 μm~100 μm of pelletizing, rotating speed during ball milling is 100 turns~400 turns/min, during ball milling mixing
Between be more than 2h.
In present embodiment, the mixed-powder is put into the powdering tank of increasing material manufacturing equipment, afterwards according to be formed
The model information of complicated shape part the mixed-powder is struck off using powdering rod so that the mixed-powder be paved with entirely into
Type face, afterwards goes out mixed-powder progress selective laser fusing sinter molding by the method that successively powdering successively sinters more
Hole silicon blank.Wherein, laser sintered power is 20W~200W, and laser scan rate is 2mm/s~7000mm/s, lift height
For 0.05mm~0.2mm.
Step 3, carries out the porous silicon base substrate reaction-sintered, nitrogenizes to obtain complicated shape nitride porous silicon member.
Specifically, the porous silicon blank is put into nitrogen sintering furnace, is passed through flowing nitrogen and carries out reaction-sintered, to obtain
Obtain complicated shape nitride porous silicon member.Wherein, the heating rate of reaction-sintered is 5 DEG C~15 DEG C/min, and nitrogen pressure is not less than
0.1MPa, and during reaction-sintered 2h is kept the temperature at 1100 DEG C, 1200 DEG C, 1300 DEG C and 1450 DEG C respectively.
The present invention is described in further detail with several embodiments below.
Embodiment 1
The preparation method for the complicated shape nitride porous silicon member that first embodiment of the invention provides comprises the following steps：
11. raw material prepares：In parts by weight prepare 80 parts of particle diameters be 1 μm silica flour, 10 parts of particle diameters be 0.01 μm oxidation
Yttrium powder and 10 parts of particle diameters are 0.01 μm of alumina powder, are put after the silica flour, the oxidation yttrium powder and alumina powder are weighed respectively
Enter in ball grinder, and carry out mechanical ball mill to obtain mixed-powder.Wherein, ball milling speed is 100 turns/min, and Ball-milling Time is
4h。
12. increasing material manufacturing：By the mixed-powder be put into used in laser gain material manufacturing equipment into material cylinder, and working
Be passed through in cabin argon gas protection after, according to complicated shape nitride porous silicon member to be formed model information by the mixed-powder by
Layer powdering simultaneously carries out selective melting using laser to powder, to obtain porous blank.Wherein, laser sintered laser power is
200W, laser scan rate 7000mm/s, lift height 0.2mm.
13. reaction-sintered：The porous body is put into nitrogen sintering furnace, is passed through flowing nitrogen, nitrogen pressure is
0.15MPa, progressively heats up by 5 DEG C/min of heating rate, and respectively in 1100 DEG C, 1200 DEG C, 1300 DEG C and 1450 DEG C insulations
2h, complicated shape nitride porous silicon member is obtained after the completion of sintering.
Embodiment 2
The preparation method for the complicated shape nitride porous silicon member that second embodiment of the invention provides mainly includes the following steps that：
21. raw material prepares：In parts by weight prepare 80 parts of particle diameters be 30 μm silica flour, 10 parts of particle diameters be 0.1 μm oxidation
The zirconia powder that iron powder and 10 parts of particle diameters are 0.1 μm, puts after the silica flour, the brown iron oxide and zirconia powder are weighed respectively
Enter and mechanical ball mill is carried out in ball grinder, to obtain mixed-powder.Wherein, ball milling speed is 100 turns/min, Ball-milling Time 2h.
22. increasing material manufacturing：By the mixed-powder be put into used in laser gain material manufacturing equipment into material cylinder, and working
Be passed through in storehouse argon gas protection after, according to complicated shape nitride porous silicon member to be formed model information by the mixed-powder by
Layer powdering simultaneously uses the mixed-powder laser power as 20W, laser scan rate 2mm/s, lift height 0.05mm
Laser sintering process successively sintered, silicon and the compound porous body of sintering aid are obtained after the completion of increasing material manufacturing.
23. reaction-sintered：The porous body is put into nitrogen sintering furnace, is passed through flowing nitrogen, nitrogen pressure is
0.15MPa, is progressively heated up by 5 DEG C/min of heating rate, and respectively at 1100 DEG C, 1200 DEG C, 1300 DEG C and 1450 DEG C
2h is kept the temperature, complicated shape nitride porous silicon member is obtained after the completion of sintering；
Embodiment 3
The preparation method for the complicated shape nitride porous silicon member that third embodiment of the invention provides mainly includes the following steps that：
31. raw material prepares：In parts by weight prepare 95 parts of particle diameters be 5 μm silica flour, 3 parts of particle diameters be 5 μm lanthana powder
And the oxidation yttrium powder that 2 parts of particle diameters are 5 μm, and put after the silica flour, the oxidation yttrium powder and the lanthana powder are weighed respectively
Enter to carry out mechanical ball mill in ball grinder to obtain mixed-powder.Wherein, ball milling speed is 400 turns/min, Ball-milling Time 4h.
32. increasing material manufacturing：By the mixed-powder be put into used in laser gain material manufacturing equipment into material cylinder, and working
Be passed through in cabin argon gas protection after, according to complicated shape nitride porous silicon member to be formed model information by the mixed-powder by
Layer powdering simultaneously uses the laser sintered work that laser power is 0.2mm for 200W, laser scan rate 7000mm/s, lift height
Skill successively sinters the mixed-powder, and silicon and the compound porous body of sintering aid are obtained after the completion of increasing material manufacturing.
33. reaction-sintered：The porous body is put into nitrogen sintering furnace, is passed through flowing nitrogen, nitrogen pressure is
0.15MPa, is progressively heated up by 5 DEG C/min of heating rate, and respectively at 1100 DEG C, 1200 DEG C, 1300 DEG C and 1450 DEG C
2h is kept the temperature, complicated shape nitride porous silicon member is obtained after the completion of sintering.
Embodiment 4
The preparation method for the complicated shape nitride porous silicon member that fourth embodiment of the invention provides mainly includes the following steps that：
41. raw material prepares：In parts by weight prepare 85 parts of particle diameters be 30 μm silica flour, 2 parts of footpaths be 10 μm zirconia powder
And the magnesia powder that 13 parts of particle diameters are 10 μm, it is put into ball after the silica flour, the zirconia powder and magnesia powder are weighed respectively
Mechanical ball mill is carried out in grinding jar to obtain mixed-powder.Wherein, ball milling speed is 400 turns/min, Ball-milling Time 6h.
42. increasing material manufacturing：By the mixed-powder be put into used in laser gain material manufacturing equipment into material cylinder, and working
Be passed through in cabin argon gas protection after, according to complicated shape nitride porous silicon member to be formed model information by the mixed-powder by
Layer powdering simultaneously uses the laser sintered work that laser power is 0.05mm for 160W, laser scan rate 800mm/s, lift height
Skill is successively sintered, and silicon and the compound porous body of sintering aid are obtained after the completion of increasing material manufacturing；
43. reaction-sintered：The porous body is put into nitrogen sintering furnace, is passed through flowing nitrogen, nitrogen pressure is
0.15MPa, is progressively heated up by 5 DEG C/min of heating rate, and respectively at 1100 DEG C, 1200 DEG C, 1300 DEG C and 1450 DEG C
2h is kept the temperature, complicated shape nitride porous silicon member is obtained after the completion of sintering.
The partial properties parameter of complicated shape nitride porous silicon member prepared by 4 embodiments of the above refers to table 1.
Table 1
The preparation method of complicated shape nitride porous silicon member provided by the invention, it uses metallic silicon and oxidesintering to help
Agent is raw material, carries out part fusing to material powder using precinct laser fusion technique and sinters, is configured to precast body, then lead to
Cross reaction-sintered nitridation method porous metals silicon precast body is changed into nitride porous silicon materials, due in material without using appoint
What high polymer binder, and the bonding of precast body melts the bonding to be formed based on metallic particles part, thus the intensity of precast body compared with
It is high and influenced without any carbon residue, it is suitable for the preparation of large complicated shape porous silicon nitride part.
As it will be easily appreciated by one skilled in the art that the foregoing is merely illustrative of the preferred embodiments of the present invention, not to
The limitation present invention, all any modification, equivalent and improvement made within the spirit and principles of the invention etc., should all include
Within protection scope of the present invention.
Claims (10)
1. a kind of preparation method of complicated shape nitride porous silicon member, it is characterised in that this method comprises the following steps：
(1) metallic silicon power of offer predetermined quality number and oxide sintering aid are as raw material；
(2) use increasing material manufacturing technique to partially sinter the raw material with it is preforming go out porous silicon base substrate；
(3) reaction-sintered is carried out to the porous silicon base substrate, complicated shape nitride porous silicon member is obtained by nitrogenizing.
2. the preparation method of complicated shape nitride porous silicon member as claimed in claim 1, it is characterised in that：The metallic silicon power
Mass fraction be 80 parts~95 parts, the mass fraction of the oxide sintering aid is 5 parts~20 parts.
3. the preparation method of complicated shape nitride porous silicon member as claimed in claim 1, it is characterised in that：The metallic silicon power
For the spherical silicon powder that average grain diameter is 1 μm~30 μm, the percentage by weight of its impurity contained is less than 1%.
4. such as the preparation method of claim 1-3 any one of them complicated shape nitride porous silicon member, it is characterised in that：It is described
Oxide sintering aid be iron oxide, ferrous oxide, yittrium oxide, lanthana, aluminium oxide, zirconium oxide and magnesia in one kind or
Person is a variety of.
5. such as the preparation method of claim 1-3 any one of them complicated shape nitride porous silicon member, it is characterised in that：It is described
The particle diameter of oxide sintering aid is 0.01 μm~10 μm, and the percentage by weight of its impurity contained is less than 0.5%.
6. such as the preparation method of claim 1-3 any one of them complicated shape nitride porous silicon member, it is characterised in that：Institute
State and the step of mechanical ball mill is carried out to the raw material is further included before raw material is sintered, rotating speed during ball milling is 100 turns~400
Turn/min, the ball milling mixing time is more than 2h.
7. such as the preparation method of claim 1-3 any one of them complicated shape nitride porous silicon member, it is characterised in that：It is described
Increasing material manufacturing technique is selective laser melting process.
8. the preparation method of complicated shape nitride porous silicon member as claimed in claim 7, it is characterised in that：Using the laser
Selective melting technique successively sinters the raw material according to the model information of complicated shape nitride porous silicon member to be formed,
Laser sintered power is 20W~200W, and laser scan rate is 2mm/s~7000mm/s, lift height for 0.05mm~
0.2mm, atmospheric condition are protected for vacuum or argon gas.
9. such as the preparation method of claim 1-3 any one of them complicated shape nitride porous silicon member, it is characterised in that：By institute
State porous silicon blank to be put into nitrogen sintering furnace, be passed through flowing nitrogen and carry out reaction-sintered, to obtain complicated shape nitride porous
Silicon member.
10. the preparation method of complicated shape nitride porous silicon member as claimed in claim 9, it is characterised in that：Reaction-sintered
Heating rate is 5 DEG C~15 DEG C/min, and nitrogen pressure is not less than 0.1MPa, and during reaction-sintered respectively 1100 DEG C, 1200 DEG C,
1300 DEG C and 1450 DEG C insulation 2h.
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| CN108947539A (en) * | 2018-09-11 | 2018-12-07 | 中国科学院上海硅酸盐研究所 | A kind of silicon nitride ceramic material and preparation method thereof for mobile phone backboard |
| CN109796208A (en) * | 2019-03-28 | 2019-05-24 | 西安增材制造国家研究院有限公司 | Si3N4Ceramic structural member and method for manufacturing same |
| CN109851370A (en) * | 2019-03-22 | 2019-06-07 | 常德科锐新材料科技有限公司 | The production method of high-intensitive high thermal conductivity silicon nitride board |
| CN110330344A (en) * | 2019-06-19 | 2019-10-15 | 华中科技大学 | A method of high porosity silicon nitride ceramics is prepared based on selective laser sintering |
| CN113563087A (en) * | 2021-07-05 | 2021-10-29 | 淄博国创中心先进车用材料技术创新中心 | Silicon nitride ceramic component and method for producing same |
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| CN108947539A (en) * | 2018-09-11 | 2018-12-07 | 中国科学院上海硅酸盐研究所 | A kind of silicon nitride ceramic material and preparation method thereof for mobile phone backboard |
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| CN110330344B (en) * | 2019-06-19 | 2020-12-18 | 华中科技大学 | Method for preparing high-porosity silicon nitride ceramic based on selective laser sintering |
| CN113563087A (en) * | 2021-07-05 | 2021-10-29 | 淄博国创中心先进车用材料技术创新中心 | Silicon nitride ceramic component and method for producing same |
| CN113563088A (en) * | 2021-07-30 | 2021-10-29 | 淄博国创中心先进车用材料技术创新中心 | Porous silicon nitride ceramic component and method for producing same |
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