CN105000889B - Method for preparing iron-containing SiCN ceramic by using precursor conversion method - Google Patents
Method for preparing iron-containing SiCN ceramic by using precursor conversion method Download PDFInfo
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- CN105000889B CN105000889B CN201510379111.2A CN201510379111A CN105000889B CN 105000889 B CN105000889 B CN 105000889B CN 201510379111 A CN201510379111 A CN 201510379111A CN 105000889 B CN105000889 B CN 105000889B
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 53
- 239000000919 ceramic Substances 0.000 title claims abstract description 43
- 238000000034 method Methods 0.000 title claims abstract description 43
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 26
- 239000002243 precursor Substances 0.000 title claims abstract description 26
- 238000006243 chemical reaction Methods 0.000 title abstract description 7
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims abstract description 38
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims abstract description 29
- 239000000843 powder Substances 0.000 claims abstract description 28
- 229920001709 polysilazane Polymers 0.000 claims abstract description 27
- XMNIXWIUMCBBBL-UHFFFAOYSA-N 2-(2-phenylpropan-2-ylperoxy)propan-2-ylbenzene Chemical compound C=1C=CC=CC=1C(C)(C)OOC(C)(C)C1=CC=CC=C1 XMNIXWIUMCBBBL-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000011259 mixed solution Substances 0.000 claims abstract description 21
- 239000000463 material Substances 0.000 claims abstract description 18
- 238000002156 mixing Methods 0.000 claims abstract description 17
- 238000000498 ball milling Methods 0.000 claims abstract description 16
- 238000000197 pyrolysis Methods 0.000 claims abstract description 12
- 238000005245 sintering Methods 0.000 claims abstract description 11
- 239000002105 nanoparticle Substances 0.000 claims description 20
- 238000010438 heat treatment Methods 0.000 claims description 17
- 238000007711 solidification Methods 0.000 claims description 14
- 230000008023 solidification Effects 0.000 claims description 14
- 238000003825 pressing Methods 0.000 claims description 9
- 238000004132 cross linking Methods 0.000 claims description 7
- 239000012467 final product Substances 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- 238000010348 incorporation Methods 0.000 claims description 2
- 238000007873 sieving Methods 0.000 claims description 2
- 238000010792 warming Methods 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 abstract description 13
- 238000005516 engineering process Methods 0.000 abstract description 6
- 238000002310 reflectometry Methods 0.000 abstract description 3
- 238000000465 moulding Methods 0.000 abstract 1
- 238000004321 preservation Methods 0.000 abstract 1
- 239000002994 raw material Substances 0.000 description 7
- 238000001723 curing Methods 0.000 description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 5
- 238000011161 development Methods 0.000 description 5
- 239000011812 mixed powder Substances 0.000 description 5
- 239000004570 mortar (masonry) Substances 0.000 description 5
- 229910010293 ceramic material Inorganic materials 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 239000011358 absorbing material Substances 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- IGHXQFUXKMLEAW-UHFFFAOYSA-N iron(2+) oxygen(2-) Chemical compound [O-2].[Fe+2].[Fe+2].[O-2] IGHXQFUXKMLEAW-UHFFFAOYSA-N 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 229920000620 organic polymer Polymers 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 239000002250 absorbent Substances 0.000 description 2
- 230000002745 absorbent Effects 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 229910000859 α-Fe Inorganic materials 0.000 description 2
- 208000033999 Device damage Diseases 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003431 cross linking reagent Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000005670 electromagnetic radiation Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000013007 heat curing Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910001092 metal group alloy Inorganic materials 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 238000000016 photochemical curing Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
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Abstract
The invention relates to a method for preparing iron-containing SiCN ceramic by using a precursor conversion method, and the method comprises the following steps: (1) uniformly mixing polysilazane, alpha-methacrylic acid and dicumyl peroxide, and obtaining a mixed solution; (2) solidifying the mixed solution; (3) carrying out crushing and ball milling of the solidified materials; (4) uniformly mixing the powder which is processed through ball milling and nanometer iron oxide; (5) carrying out prepressing and molding of the obtained powder, and obtaining a green compact; (6) carrying out pyrolysis/sintering and heat preservation of the green compact obtained in the step (5) at 1000-1400 DEG C; obtaining the product. The iron-containing SiCN ceramic prepared by the precursor conversion method has the advantages of simple preparation technology and excellent high temperature performance; the dielectric constant value is obviously increased by introducing nanometer iron oxide, and the dielectric loss is correspondingly increased; the electromagnetic attenuation coefficient of the ceramic is increased, and the reflectivity is increased.
Description
Technical field
The present invention relates to the preparation method of iron content silicon carbonitride ceramic, and in particular to a kind of presoma conversion method synthesizes iron content silicon
The method of C-N ceramic, belongs to field of inorganic nonmetallic material.
Background technology
With the arriving and the fast development of diversified intelligence science and technology of information age, data transfer, telecommunications, nothing
Line network system, satellite launch, system diagnostics and detection, radar etc. are employed to and launch electromagnetic wave, the electricity of different emission sources
Magnetic wave always interferes the accuracy reduction for causing transmission data, and the interference of external electromagnetic wave even can cause electronic device
Failure and damage, therefore electromagnetic radiation pollution turns into current research problem demanding prompt solution.But by simple electromagnetic shielding
Can not fundamentally weaken, eliminate electromagnetic wave, the energy of electromagnetic wave is changed into other forms using electromagnetic wave absorbent material
Energy (such as mechanical energy, heat energy and electric energy) utilize or dissipate, help at utmost to eliminate the influence of electromagnetic wave.
With reference to the electromagenetic wave radiation pollution problem for appearing above, thickness of thin, lightweight, absorption band are wide and absorption intensity is high
Electromagnetic wave absorbent material gradually causes the extensive interest of people.
Traditional absorbing material mainly including ferrite, metal alloy, graphite and silicon carbide ceramics etc., with suction higher
Intensity of wave, but its absorption band is not wide and density is larger.Especially ferrite and traditional ceramics class absorbing material due to density it is big
The reason for limit its further development in the field, therefore structure is similar and the precursor ceramic of relative lightweight is inhaling ripple material
There is potential application value in material.
Precursor ceramic (Polymer-Derived Ceramics) is directly to be pyrolyzed organic polymer presoma and obtain
The ceramic material for arriving.Presoma pyrolysismethod is a kind of new ceramic preparation technology, incomparable with traditional ceramics technique
Many merits.Directly in a mold can be molded liquid organic precursor through photocuring or heat cure by the preparation of precursor ceramic
Afterwards, pyrolysis sintering is obtained, and is conducive to preparing complex-shaped device, film, fiber or porous article, is beaten in MEMS, catalysis, 3D
There is vast potential for future development in the fields such as print, therefore its appearance causes the favor of material researcher and obtains rapid immediately
Development.Precursor ceramic technology is related to, using precursor oligomer or polymer is chemically synthesized, then be molded, crack
To ceramics, the frontier that inorganic ceramic is prepared from organic polymer is started, has realized the revolutionary innovation of ceramic preparation technology,
The advantage of collection organic polymer and ceramic two big materials, revolutionary innovation is made to traditional ceramics technique.
Because SiCN precursor ceramics have unique non crystalline structure, homogeneous chemical composition and good thermal shock resistance
And high temperature oxidation resistance, correlative study is also increasingly valued by people.But, current SiCN precursors ceramics are inhaled in microwave
Debit face performance is not good, its development in absorbing material field is significantly limited.
The content of the invention
In view of the shortcomings of the prior art, the present invention provides a kind of method that precursor process prepares iron content SiCN ceramics, the party
Method process is simple, low production cost, short preparation period, obtained sample electromagnetic wave attenuation coefficient are high, and microwave absorbing property is good.
Technical solution of the present invention is as follows：
A kind of method that precursor process prepares iron content SiCN ceramics, including step is as follows：
(1) batch mixing：In N2It is under atmosphere, the stirring of polysilazane (PSZ), α-methacrylic acid and cumyl peroxide is equal
It is even, obtain mixed solution；
The polysilazane：Cumyl peroxide in mass ratio 96%~98%：2%~4% dispensing, the Alpha-Methyl
Acrylic acid is the 10%~20% of polysilazane and cumyl peroxide gross mass；
(2) crosslinking curing：By step (1) gained mixed solution 3~5 DEG C/min heating rate from room temperature to
500~700 DEG C, solidify 2~6h；
(3) ball milling is crushed：Crushing material ball milling obtained by step (2) is solidified, crosses 100-200 mesh sieves；
(4) batch mixing：Powder obtained by step (3) sieving is added into nano-sized iron oxide and is well mixed；
The nano-sized iron oxide mixes dispensings by the 20~100% of step (3) gained powder quality；
(5) granulating and forming：By step (4) gained powder compressing, isostatic cool pressing under the pressure of 10MPa~30MPa,
Obtain green compact；
(6) pyrolysis/sintering：By step (5) gained green compact in N2Temperature under atmosphere protection at 1000 DEG C~1400 DEG C is entered
Row pyrolysis/sintering, is incubated 2h~4h, obtains final product.
, according to the invention it is preferred to, the polysilazane described in step (1) is HTT1800.HTT1800 can market buy,
Also can be prepared by prior art oneself.
, according to the invention it is preferred to, heating rate is 3 DEG C/min, 600 DEG C of solidification temperature, hardening time in step (2)
4h.Relatively low heating rate and hardening time higher, to ensure the full cross-linked solidification of polysilazane, promote the carrying out of reaction.
, according to the invention it is preferred to, nano-sized iron oxide described in step (4) is by the 30~100% of step (3) resulting material
Mix dispensing, further preferred 30%, 60%, 80%, 100%.
, according to the invention it is preferred to, isostatic cool pressing is carried out under 180MPa in step (5), pressurize 300s.
, according to the invention it is preferred to, in step (6) from room temperature with 3~5 DEG C/min heating rates be warming up to 1000 DEG C~
1400 DEG C be pyrolyzed/sinter；It is further preferred that pyrolysis temperature is 1300 DEG C.
Principle of the invention：
The present invention with polysilazane be presoma originate, cumyl peroxide as crosslinking agent, can be distributed in double gas
Preparation SiCN ceramic materials are mixed under the assistance of device (vacuum/inertia branch manifold system, be commonly called as Schlenk line), in original
The material mixed dissolution stage introduces carbon source methacrylic acid and phosphorus content SiCN ceramic materials higher is obtained, and the raw material doping stage introduces
Source of iron nano-sized iron oxide, is obtained magnetic property preferable SiCN (Fe) precursor ceramic material.
Beneficial effects of the present invention：
1st, the present invention prepares the SiCN ceramics of iron content by precursor process, and introducing nano-sized iron oxide can make dielectric constant values bright
Aobvious to increase, dielectric loss also accordingly increases；Its electromagnetic attenuation coefficient also increases, and reflectivity is improved.
2nd, the present invention uses presoma conversion method, and preparation process is simple, resulting materials resistance to elevated temperatures is excellent.
Brief description of the drawings
Fig. 1 is the SEM photograph of the iron content SiCN ceramics samples obtained by the embodiment of the present invention 1.
Specific embodiment
Technical scheme is described further with reference to embodiment, but institute's protection domain of the present invention is not limited to
This.
Raw materials used in embodiment to be convenient source, device therefor is conventional equipment, commercial products.
Embodiment 1：
A kind of precursor process preparation iron content SiCN ceramic methods, including step is as follows：
(1) batch mixing：In N2Under atmosphere, polysilazane 9.6g, α-methacrylic acid 2g, cumyl peroxide are weighed
0.4g, stirs 2h in constant temperature blender with magnetic force, obtains mixed solution；
Polysilazane in mixed solution：Cumyl peroxide in mass ratio 96%：4% dispensing, α-methacrylic acid is
The 20% of polysilazane and cumyl peroxide gross mass；
(2) crosslinking curing：By step (1) gained mixed solution 3 DEG C/min heating rate from room temperature to 600 DEG C
Solidification 2h；
(3) ball milling is crushed：Material obtained by step (2) solidification is crushed into ball milling in vibrator, 100 mesh sieves are crossed；
(4) batch mixing：Weigh nano-sized iron oxide 0.15g and step (3) gained powder 0.5g be well mixed in agate mortar,
Mixed powder is obtained, nano-sized iron oxide is that mass ratio is 3 with step (3) gained powder in powder：10 raw material；
(5) granulating and forming：Step (4) gained powder is fitted into mould, single shaft is compressing under the pressure of 10MPa,
180MPa isostatic cool pressings, pressurize 300s obtains green compact；
(6) pyrolysis/sintering：Step (5) gained green compact are fitted into tube furnace, in N2In 1000 DEG C of temperature under atmosphere protection
Degree be pyrolyzed/sinter, 3 DEG C/min of heating rate, is incubated 4h, is obtained final product.
The SEM photograph of iron content SiCN ceramics samples obtained in the present embodiment is as shown in figure 1, as shown in Figure 1, obtained contains
Iron SiCN ceramics samples occur without crystalline phase, and typical unformed shape pattern is presented.
Embodiment 2：
A kind of precursor process preparation iron content SiCN ceramic methods, including step is as follows：
(1) batch mixing：In N2Under atmosphere, polysilazane 9.6g, α-methacrylic acid 1g, cumyl peroxide are weighed
0.4g, stirs 2h in constant temperature blender with magnetic force, obtains mixed solution；
Polysilazane in mixed solution：Cumyl peroxide in mass ratio 96%：4% dispensing, α-methacrylic acid is
The 10% of polysilazane and cumyl peroxide gross mass；
(2) crosslinking curing：By step (1) gained mixed solution 5 DEG C/min heating rate from room temperature to 600 DEG C
Solidification 2h；
(3) ball milling is crushed：Material obtained by step (2) solidification is crushed into ball milling in vibrator, 200 mesh sieves are crossed；
(4) batch mixing：Nano-sized iron oxide 0.3g is weighed, step (3) gained powder 0.5g is well mixed in agate mortar, obtains
To mixed powder, nano-sized iron oxide is that mass ratio is 3 with step (3) gained powder in powder：5 raw material；
(5) granulating and forming：Step (4) gained powder is fitted into mould, single shaft is compressing under the pressure of 10MPa,
180MPa isostatic cool pressings, pressurize 300s obtains green compact；
(6) pyrolysis/sintering：Step (5) gained green compact are fitted into tube furnace, in N2In 1100 DEG C of temperature under atmosphere protection
Degree is pyrolyzed, 5 DEG C/min of heating rate, is incubated 4h, is obtained final product.
Embodiment 3：
A kind of SiCN ceramic methods of precursor process preparation iron content, including step is as follows：
(1) batch mixing：In N2Under atmosphere, polysilazane 9.6g, α-methacrylic acid 1g, cumyl peroxide are weighed
0.4g, stirs 2h in constant temperature blender with magnetic force, obtains mixed solution；
Polysilazane in mixed solution：Cumyl peroxide in mass ratio 96%：4% dispensing, α-methacrylic acid is
The 10% of polysilazane and cumyl peroxide gross mass；
(2) crosslinking curing：By step (1) gained mixed solution 5 DEG C/min heating rate from room temperature to 600 DEG C
Solidification 2h；
(3) ball milling is crushed：Material obtained by step (2) solidification is crushed into ball milling in vibrator, 100 mesh sieves are crossed；
(4) batch mixing：Nano-sized iron oxide iron 0.4g is weighed, step (3) gained powder 0.5g is well mixed in agate mortar
Mixed powder is obtained, nano-sized iron oxide iron is that mass ratio is 4 with step (3) gained powder in powder：5 raw material；
(5) granulating and forming：Step (4) gained powder is fitted into mould, single shaft is compressing under the pressure of 10MPa,
180MPa isostatic cool pressings, pressurize 300s obtains green compact；
(6) pyrolysis/sintering：Step (5) gained green compact are fitted into tube furnace, in N2In 1200 DEG C of temperature under atmosphere protection
Degree is pyrolyzed, 5 DEG C/min of heating rate, is incubated 4h, is obtained final product.
Embodiment 4：
A kind of precursor process preparation iron content SiCN ceramic methods, including step is as follows：
(1) batch mixing：In N2Under atmosphere, polysilazane 9.8g, α-methacrylic acid 2g, cumyl peroxide are weighed
0.2g, stirs 2h in constant temperature blender with magnetic force, obtains mixed solution；
Polysilazane in mixed solution：Cumyl peroxide in mass ratio 98%：2% dispensing, α-methacrylic acid is
The 20% of polysilazane and cumyl peroxide gross mass；
(2) crosslinking curing：By step (1) gained mixed solution 3 DEG C/min heating rate from room temperature to 500 DEG C
Solidification 2h；
(3) ball milling is crushed：Material obtained by step (2) solidification is crushed into ball milling in vibrator, 150 mesh sieves are crossed；
(4) batch mixing：Nano-sized iron oxide iron 0.5g is weighed, step (3) gained powder 0.5g is well mixed in agate mortar
Mixed powder is obtained, nano-sized iron oxide is that mass ratio is 1 with step (3) gained powder in powder：1 raw material；
(5) granulating and forming：Step (4) gained powder is fitted into mould, single shaft is compressing under the pressure of 10MPa,
180MPa isostatic cool pressings, pressurize 300s obtains green compact；
(6) pyrolysis/sintering：Step (5) gained green compact are fitted into tube furnace, in N2In 1300 DEG C of temperature under atmosphere protection
Degree is pyrolyzed, 3 DEG C/min of heating rate, is incubated 4h, is obtained final product.
Embodiment 5：
A kind of precursor process preparation iron content SiCN ceramic methods, including step is as follows：
(1) batch mixing：In N2Under atmosphere, polysilazane 9.8g, α-methacrylic acid 2g, cumyl peroxide are weighed
0.2g, stirs 2h in constant temperature blender with magnetic force, obtains mixed solution；
Polysilazane in mixed solution：Cumyl peroxide in mass ratio 98%：2% dispensing, α-methacrylic acid is
The 20% of polysilazane and cumyl peroxide gross mass；
(2) crosslinking curing：By step (1) gained mixed solution 3 DEG C/min heating rate from room temperature to 700 DEG C
Solidification 2h；
(3) ball milling is crushed：Material obtained by step (2) solidification is crushed into ball milling in vibrator, 100 mesh sieves are crossed；
(4) batch mixing：Nano-sized iron oxide 0.5g is weighed, step (3) gained powder 0.5g is well mixed in agate mortar
Mixed powder is obtained, nano-sized iron oxide is that mass ratio is 1 with step (3) gained powder in powder：1 raw material；
(5) granulating and forming：Step (4) gained powder is fitted into mould, single shaft is compressing under the pressure of 10MPa,
180MPa isostatic cool pressings, pressurize 300s obtains green compact；
(6) pyrolysis/sintering：Step (5) gained green compact are fitted into tube furnace, in N2In 1400 DEG C of temperature under atmosphere protection
Degree is sintered, 3 DEG C/min of heating rate, is incubated 4h, obtains final product.
Comparative example
As described in Example 1, difference is to leave out step (3) mixing process, does not mix nano-sized iron oxide.
Experimental example
By iron content SiCN ceramics and SiCN ceramics obtained in comparative example obtained in embodiment 1~5, test dielectric constant, Jie
Electrical loss, electromagnetic attenuation coefficient, reflectivity and heat resistance, as a result as shown in table 1.
Table 1
| Numbering index | Dielectric constant | Magnetic loss | Magnetic conductivity | Electromagnetic attenuation coefficient |
| Embodiment 1 | 2.03 | 4.3 | 1.14 | 354 |
| Embodiment 2 | 2.16 | 4.6 | 1.25 | 361 |
| Embodiment 3 | 2.5 | 5.2 | 1.36 | 451 |
| Embodiment 4 | 2.8 | 6.1 | 1.43 | 625 |
| Embodiment 5 | 3.2 | 6.5 | 1.58 | 800 |
| Comparative example 1 | ~ | 2.5 | 0.83 | 256 |
As shown in Figure 1, the absorbing property of the iron content SiCN ceramics for being obtained after present invention incorporation nano-sized iron oxide is excellent.Introduce
Nano-sized iron oxide makes dielectric constant values substantially increase, and dielectric loss also accordingly increases；Its electromagnetic attenuation coefficient also increases.
It should be noted that listed above is only several specific embodiments of the invention, it is clear that the present invention is not only
It is limited to above example, there can also be other to deform.Those skilled in the art directly derived from the disclosure of invention or
All deformations of amplification are connect, protection scope of the present invention is considered as.
Claims (6)
1. a kind of method that precursor process prepares iron content SiCN ceramics, including step is as follows：
（1）Batch mixing：In N2Under atmosphere, by polysilazane（PSZ）, α-methacrylic acid and cumyl peroxide stir, obtain
To mixed solution；
The polysilazane：Cumyl peroxide in mass ratio 96% ~ 98%：2% ~ 4% dispensing, the Alpha-Methyl
Acrylic acid is the 10% ~ 20% of polysilazane and cumyl peroxide gross mass；
（2）Crosslinking curing：By step（1）Gained mixed solution 3 ~ 5 DEG C/min heating rate from room temperature
To 500 ~ 700 DEG C, solidify 2 ~ 6h；
（3）Crush ball milling：By step（2）Crushing material ball milling obtained by solidification, crosses 100 mesh sieves；
（4）Batch mixing：By step（3）Powder obtained by sieving adds nano-sized iron oxide and is well mixed；
The nano-sized iron oxide presses step（3）30 ~ 60% incorporation dispensings of gained powder quality；
（5）Granulating and forming：By step（4）Gained powder is compressing under the pressure of 10MPa ~ 30MPa, isostatic cool pressing, obtains
Green compact；
（6）Pyrolysis/sintering：By step（5）Gained green compact are in N2Temperature under atmosphere protection at 1000 DEG C ~ 1400 DEG C be pyrolyzed/
Sintering, is incubated 2h ~ 4h, obtains final product.
2. the method that precursor process according to claim 1 prepares iron content SiCN ceramics, it is characterised in that step（1）In
Described polysilazane is HTT1800.
3. the method that precursor process according to claim 1 prepares iron content SiCN ceramics, it is characterised in that step（2）In
Heating rate is 3 DEG C/min, 600 DEG C of solidification temperature, hardening time 4h.
4. the method that precursor process according to claim 1 prepares iron content SiCN ceramics, it is characterised in that step（5）In
Isostatic cool pressing is carried out under 180 MPa, pressurize 300s.
5. the method that precursor process according to claim 1 prepares iron content SiCN ceramics, it is characterised in that step（6）In
Being warming up to 1000 DEG C ~ 1400 DEG C with 3 ~ 5 DEG C/min heating rates from room temperature be pyrolyzed/sinter.
6. the method that precursor process according to claim 1 prepares iron content SiCN ceramics, it is characterised in that step（6）In
Pyrolysis temperature is 1300 DEG C.
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| CN106495700B (en) * | 2016-10-26 | 2019-06-21 | 山东大学 | A kind of method that presoma conversion method prepares SiCN (Fe) precursor ceramic of rare earth doped oxide |
| CN107555999A (en) * | 2017-09-29 | 2018-01-09 | 山东大学 | A kind of preparation method for the iron content silicon-carbon nitrogen precursor ceramic for adulterating europium oxide |
| CN109702853B (en) * | 2019-01-24 | 2020-05-01 | 青岛大学 | 3D printing method of magnetic ceramic and magnetic ceramic prepared by method |
| CN112321318A (en) * | 2020-10-20 | 2021-02-05 | 上海航翼高新技术发展研究院有限公司 | Polymer precursor porous magnetic ceramic system based on 3D printing technology and preparation method thereof |
| CN116409999B (en) * | 2023-03-22 | 2024-05-28 | 南京信息工程大学 | S-band silicon-carbon-nitrogen ceramic wave-absorbing material and preparation method thereof |
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