CN106495700A - A kind of presoma conversion method prepares the SiCN of rare earth doped oxide（Fe）The method of precursor ceramic - Google Patents

A kind of presoma conversion method prepares the SiCN of rare earth doped oxide（Fe）The method of precursor ceramic Download PDF

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CN106495700A
CN106495700A CN201610962212.7A CN201610962212A CN106495700A CN 106495700 A CN106495700 A CN 106495700A CN 201610962212 A CN201610962212 A CN 201610962212A CN 106495700 A CN106495700 A CN 106495700A
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rare earth
sicn
powder
earth doped
precursor ceramic
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CN106495700B (en
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龚红宇
刘玉
张玉军
冯玉润
郭学
林骁
周立伟
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Shandong University
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Abstract

The present invention relates to a kind of method containing ferromagnetism silicon carbonitride ceramic of presoma conversion method synthesizing blender rare earth oxide.It is as follows that the method comprising the steps of：(1) polysilazane, α methacrylic acids and cumyl peroxide are mixed, obtains mixed solution；(2) mixed solution is solidified；(3) solidify the pre-milled material for obtaining, crushing ball milling, sieve, obtain powder granule；(4) alpha-iron oxide nano-powder and RE oxide powder are added in powder granule, obtains mixed material；(5) mixed material is compressing, isostatic cool pressing, pressurize obtain green compact；(6) temperature by gained green compact at 1000 DEG C 1400 DEG C is sintered, and is obtained final product.The method process is simple, low production cost, short preparation period, obtained product electromagnetic wave attenuation coefficient are high, and microwave absorbing property is good.

Description

A kind of presoma conversion method prepares SiCN (Fe) the presoma pottery of rare earth doped oxide The method of porcelain
Technical field
The present invention relates to the preparation method of SiCN (Fe) precursor ceramic of rare earth doped oxide, and in particular to Yi Zhongqian The method containing ferromagnetism silicon carbonitride ceramic of body conversion method synthesizing blender rare earth oxide is driven, belongs to Inorganic Non-metallic Materials neck Domain.
Background technology
With the development of science and technology, electromagenetic wave radiation has become a big harm, not only periodic traffic and electronic system is made Into infringement, health can be also damaged.And the progress of Detection Techniques so that in modern war, realize that target is stealthy, it is military to improve The existence of device change system and penetration ability have profound significance, and therefore electromangnetic spectrum just seems particularly significant.And it is electric The incident electromagnetic wave of electro-magnetic wave absorption material absorbable, decay, and convert electromagnetic energy into heat energy and dissipate, or make electromagnetic wave because Interfere and cancellation, therefore electromagnetic wave absorbent material becomes study hotspot in recent years.
More typical traditional absorbing material, such as ferrite, graphite etc., with absorb by force, low cost, frequency band wider etc. excellent Point, but at the same time, it may have the shortcomings of high-temperature behavior is poor, density is big, therefore limit its further development in the field. And the ceramic material such as SiCN, mullite, absorbing property is more preferable, and the energy of radar wave can be effectively lost.
Precursor ceramic (Polymer-Derived Ceramics (PDCs)) is will be directly hot for organic polymer presoma Ceramic material obtained from solution, can by change presoma chemical composition and technique come change precursor ceramic structure and Composition.Using presoma pyrolysismethod pottery preparation technology, can be directly by liquid organic precursor in a mold through photocuring or heat After curing molding, pyrolysis sintering obtains the pottery of specific form structure, and product has the microstructure of stable homogeneous.
The SiCN precursor ceramics prepared using this presoma conversion method are a kind of dielectric loss type absorbing materials, because of which The excellent mechanical performance such as high intensity, high-moduluss, high rigidity, low-density, heat resistance, chemically stable, oxidation resistance etc. and Extensive concern is at home and abroad received.And other elements M (B, Al, Fe, Co, Mo is further introduced in SiCN precursor ceramics Deng), SiCN (M) precursor ceramic is obtained, ceramic electromagnetic performance can be improved.And why absorbing property is greatly promoted, be because For more meeting to absorbing material two big requirements：Impedance matching (ripple enters wave-absorber and do not reflect) and loss (inhale ripple material Material has enough lossies to the ripple that injects).Introducing Fe sources preparation SiCN (Fe) precursor ceramic has obtained widely studied at present.
Chinese patent literature CN 105000889A discloses the side that a kind of presoma conversion method prepares iron content silicon carbonitride ceramic Method.It is as follows that the method comprising the steps of：(1) by polysilazane, α-methacrylic acid, cumyl peroxide mix homogeneously, obtain mixed Close solution；(2) mixed solution is solidified；(3) solidify the crushing material ball milling of gained；(4) by ball milling after powder and nano oxygen Change ferrum mix homogeneously；(5) by gained powder pre-molding, green compact are obtained；(6) by step (5) gained green compact at 1000 DEG C -1400 DEG C Temperature carry out being pyrolyzed/sintering, insulation is obtained final product.The method preparation process is simple, resulting materials high-temperature behavior are excellent, with certain Absorbing property, but absorbing property is not good enough.
Chinese patent literature CN 104944960A discloses a kind of presoma conversion method and prepares the nitrogen of silicon-carbon containing ferric acetyl acetonade The method of pottery.Comprise the following steps：(1) by polysilazane, α-methacrylic acid, cumyl peroxide mix homogeneously, obtain Mixed solution；(2) mixed solution is solidified；(3) by the crushing material ball milling of solidification gained；(4) by powder and ferric acetyl acetonade Mix homogeneously；(5) by the powder pre-molding of mix homogeneously, green compact are obtained；(6) green compact are carried out in 1000 DEG C -1400 DEG C of temperature Pyrolysis/sintering, insulation are obtained final product.The material at high temperature performance that this invention is prepared is good, with certain microwave absorbing property, but Assimilation effect is not good enough.
Rare earth element is the element that a class has the not paired 4f electronics shielded by outermost electron, with magnetic moment, and not The transition elements such as Fe, Co, Ni are same as, they are affected by the surrounding environment less, and the interaction with surrounding is indirectly to hand over The effect of changing, so that have the Net magnetic moment not being cancelled.So, rare earth has good paramagnetic susceptibility, saturation magnetization, magnetocrystalline Anisotropy and magnetostriction.Therefore, based on the special electronic structure of rare earth element and electromagnetic performance, can be with rare earth oxide As dopant, it is incorporated in other absorbing materials, further enhances the absorbing property of material.
Content of the invention
For the deficiencies in the prior art, the present invention provides the SiCN that a kind of presoma conversion method prepares rare earth doped oxide (Fe) method of precursor ceramic.The method process is simple, low production cost, short preparation period, obtained product electromagnetic wave Attenuation quotient is high, and microwave absorbing property is good.
Technical scheme is as follows：
A kind of method that presoma conversion method prepares SiCN (Fe) precursor ceramic of rare earth doped oxide, including step As follows：
(1) batch mixing：Under an inert atmosphere, polysilazane, α-methacrylic acid and cumyl peroxide are mixed 1-2h, obtains mixed solution；
The polysilazane：The mass ratio of cumyl peroxide is 96-98：2-4；The addition of the α-methacrylic acid Measure as polysilazane and the 10%-20% of cumyl peroxide gross mass；
(2) crosslinking curing：By step (1) gained mixed solution at 400 DEG C -600 DEG C, under vacuum condition, solidify 2-4h；
(3) ball milling is crushed：Material that step (2) crosslinking curing is obtained is pre-milled, crush ball milling, sieve, and obtains powder Body granule；
(4) batch mixing：Alpha-iron oxide nano-powder, mix homogeneously is added to obtain mixed powder in the powder granule obtained to step (3) Body；RE oxide powder is subsequently adding, mix homogeneously obtains mixed material；
(5) granulating and forming：Will be compressing for step (4) gained mixed material, isostatic cool pressing, pressurize obtain green compact；
(6) pyrolysis/sintering：By step (5) gained green compact under inert gas shielding, in 1000 DEG C -1400 DEG C of temperature Sintering 2-4h, obtains final product SiCN (Fe) precursor ceramic of rare earth doped oxide.
, according to the invention it is preferred to, in step (1), polysilazane is HTT1800.HTT1800 can market buy, Can prepare by prior art；Described α-methacrylic acid is referred to as MA, and described cumyl peroxide is referred to as DCP.
, according to the invention it is preferred to, polysilazane in step (1)：The mass ratio of cumyl peroxide is 98：2.
, according to the invention it is preferred to, in step (1), inert atmosphere is nitrogen, argon or helium atmosphere.
, according to the invention it is preferred to, in step (2), heating rate is 2-5 DEG C/min；Solidification temperature 500-600 DEG C, Hardening time 3-4h；Preferably, heating rate is 3-4 DEG C/min.Relatively low heating rate and higher hardening time are ensureing The full cross-linked solidification of polysilazane, promotes the carrying out of reaction.
, according to the invention it is preferred to, the quality of nano-sized iron oxide and step (3) gained powder granule in step (4) Than for 40-60：40-60.
, according to the invention it is preferred to, the addition of step (4) middle rare earth is the 2%- of mixed powder quality 40%；Preferably, 10%-30% of the addition of rare earth oxide for mixed powder quality；It is further preferred that rare-earth oxidation The addition of thing for mixed powder quality 5%.
, according to the invention it is preferred to, step (4) middle rare earth is Dy2O3、Eu2O3、Sm2O3、Y2O3Or Gd2O3.
It is further preferred that the rare earth oxide is Eu2O3.
, according to the invention it is preferred to, compressing under the pressure of 10MPa in step (5)；Preferably, the step Suddenly in (5), isostatic cool pressing is carried out under 180MPa, pressurize 300s.
, according to the invention it is preferred to, in step (6), noble gases are nitrogen, argon or helium.
, according to the invention it is preferred to, in step (6), heating rate is 3-5 DEG C/min.
The principle of the present invention：
SiCN precursor ceramic materials have excellent dielectric properties, introduce source of iron, can make in SiCN precursor ceramics Its dielectric loss increases, and increased magnetic loss, realizes loss mechanisms diversification.On this basis, using rare earth element Special electronic structure and electromagnetic performance, a certain amount of rare earth oxide are mixed in SiCN (Fe) absorbing material matrix, can be adjusted Section, the electromagnetic parameter for optimizing absorbing material, reach the purpose for further improving Absorbing Materials.
Due to compared to other sources of iron, Fe2O3Addition larger to the dielectric loss of material and the impact of magnetic loss.Therefore The present invention is with dopen Nano Fe2O3SiCN (Fe) precursor ceramic as matrix.
Rare earth element is different from the transition elements such as Fe, Co, Ni, with good paramagnetic susceptibility, saturation magnetization, magnetic Anisotropic crystalline and magnetostriction.A certain amount of rare earth oxide is mixed in SiCN (Fe) precursor ceramic, material magnetic can be changed Media property and dielectric properties so as to the imaginary part increase of the imaginary part and complex dielectric permittivity of complex permeability, promote magnetic loss and dielectric The increase of loss.The incorporation of rare earth oxide also improves the magnetic anisotropy of absorbing material, on the basis of SiCN (Fe), not only Absorbing property is improve, and more efficiently improves the microwave absorbing property of material.
Beneficial effects of the present invention are as follows：
1st, the present invention prepares SiCN (Fe) precursor ceramic of rare earth doped oxide by presoma conversion method, and molding is good Well, there is some strength, on the basis of nano-sized iron oxide being introduced in SiCN precursor ceramics, be further doped with rare-earth oxidation Thing, using the special electronic structure of rare earth oxide and electromagnetic performance, it will be apparent that improves the microwave absorbing property of SiCN potteries, carries Its electromagnetic wave attenuation coefficient high.
2nd, the present invention adopts presoma conversion method, and preparation temperature is low, and preparation method is simple, low production cost, manufacturing cycle Short, resulting materials chemical stability, high-temperature behavior are good.
Description of the drawings
Fig. 1 is that the X ray of SiCN (Fe) precursor ceramic of the rare earth doped oxide obtained by the embodiment of the present invention 1 spreads out Penetrate collection of illustrative plates.
Fig. 2 is that the SEM of SiCN (Fe) precursor ceramic of the rare earth doped oxide obtained by the embodiment of the present invention 1 shines Piece.
The frequency of SiCN (Fe) precursor ceramic of rare earth doped oxides of the Fig. 3 obtained by the embodiment of the present invention 1-anti- Penetrate rate R change curve.
Fig. 4 is the frequency-electricity of SiCN (Fe) precursor ceramic of the rare earth doped oxide obtained by the embodiment of the present invention 1 Magnetic attenuation quotient a change curves.
Fig. 5 is the frequency-reflection of SiCN (Fe) precursor ceramic of the rare earth doped oxide obtained by embodiment 1,2,3 Rate R change curve comparison diagram.
Fig. 6 is the frequency-reflection of SiCN (Fe) precursor ceramic of the rare earth doped oxide obtained by embodiment 4,5,6 Rate R change curve comparison diagram.
Fig. 7 is the frequency-reflection of SiCN (Fe) precursor ceramic of the rare earth doped oxide obtained by embodiment 7,8,9 Rate R change curve comparison diagram.
Fig. 8 is the frequency-electromagnetism of SiCN (Fe) precursor ceramic of the rare earth doped oxide obtained by embodiment 1,2,3 Attenuation quotient a change curve comparison diagrams.
Fig. 9 is the frequency-electromagnetism of SiCN (Fe) precursor ceramic of the rare earth doped oxide obtained by embodiment 4,5,6 Attenuation quotient a change curve comparison diagrams.
Figure 10 is the frequency-electricity of SiCN (Fe) precursor ceramic of the rare earth doped oxide obtained by embodiment 7,8,9 Magnetic attenuation quotient a change curve comparison diagrams.
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 be convenient source, device therefor is conventional equipment, commercial products.
Polysilazane used is HTT1800, and commercial products, from Shanghai Hai Yi scientific ＆ trading Co., Ltd.s.
Embodiment 1
A kind of method that presoma conversion method prepares SiCN (Fe) precursor ceramic of rare earth doped oxide, including step As follows：
(1) batch mixing：In N2Under atmosphere, polysilazane 9.8g, α-methacrylic acid 2g, cumyl peroxide is weighed 0.2g, adds in reaction bulb, stirs 1h, obtain single transparent mixed solution in constant temperature blender with magnetic force；
Polysilazane in the mixed solution：The mass ratio of cumyl peroxide is 98：2, the α-methacrylic acid Addition be the 20% of polysilazane and cumyl peroxide gross mass；
(2) crosslinking curing：Step (1) gained mixed solution is heated in vacuum tube furnace and is allowed to crosslinking curing, from room Temperature is warming up to 600 DEG C of solidification 4h, and temperature rate is 3 DEG C/min；
(3) ball milling is crushed：The material that step (2) crosslinking curing is obtained is taken, precomminution in agate mortar, then in vibration Ball milling is crushed in ball mill, 100 mesh sieves is crossed, is obtained powder granule；
(4) batch mixing：Take the powder granule 10.5g of step (3) gained, add alpha-iron oxide nano-powder 9.5g, mix homogeneously, Obtain mixed powder；
In the mixed powder, nano-sized iron oxide is 47.5 with the mass ratio of step (3) gained powder granule：52.5；
By 1g Eu2O3Powder body is added in the mixed powder of above-mentioned gained, and mix homogeneously in agate mortar obtains mixture Material；The Eu2O3The quality of powder body for mixed powder quality 5%；
(5) granulating and forming：Step (4) gained mixed material is loaded in mould, under the pressure of 10MPa, single shaft is pressed into Type, then under 180MPa isostatic cool pressings, pressurize 300s obtains green compact；
(6) pyrolysis/sintering：Step (5) gained green compact are loaded in tube furnace, in N2Under atmosphere protection, at 1000 DEG C Temperature is pyrolyzed 4h, 3 DEG C/min of heating rate, obtains final product SiCN (Fe) precursor ceramic of rare earth doped oxide.
SiCN (Fe) the precursor ceramic test X-ray diffractogram of the rare earth doped oxide that the present embodiment is prepared Spectrum, SEM photograph, frequency-reflectance R and frequency-electromagnetic attenuation coefficient a change curve Comparative maps, as shown in Figure 1,2,3, 4.
As shown in Figure 1, in obtained product in addition to containing Fe, also containing the rare earth oxide for having adulterated.
As shown in Figure 2, the incorporation of rare earth oxide is little to the structural change of SiCN (Fe) precursor ceramics, final product point Scattered property is good, without crystal grain adhesion agglomeration.
From Fig. 3,4, with the increase of frequency, reflectance is in reduction trend, and electromagnetic attenuation coefficient is in increase tendency, i.e., Sample electromagnetic wave absorption performance increases with the increase of frequency.Reflectance reaches minimum -18 at the 16.6GHz, and electromagnetic attenuation Coefficient also reaches maximum 653 at 16.1GHz.It follows that prepared material has excellent absorbing property.
Embodiment 2
A kind of method that presoma conversion method prepares SiCN (Fe) precursor ceramic of rare earth doped oxide, including step As follows：
(1) batch mixing：In N2Under atmosphere, polysilazane 9.8g, α-methacrylic acid 2g, cumyl peroxide is weighed 0.2g, adds in reaction bulb, stirs 1h, obtain single transparent mixed solution in constant temperature blender with magnetic force；
Polysilazane in the mixed solution：The mass ratio of cumyl peroxide is 98：2, the α-methacrylic acid Addition be the 20% of polysilazane and cumyl peroxide gross mass；
(2) crosslinking curing：Step (1) gained mixed solution is heated in vacuum tube furnace and is allowed to crosslinking curing, from room Temperature is warming up to 600 DEG C of solidification 4h, and temperature rate is 5 DEG C/min；
(3) ball milling is crushed：The material that step (2) crosslinking curing is obtained is taken, precomminution in agate mortar, then in vibration Ball milling is crushed in ball mill, 100 mesh sieves is crossed, is obtained powder granule；
(4) batch mixing：Take the powder granule 10.5g of step (3) gained, add alpha-iron oxide nano-powder 9.5g, mix homogeneously, Obtain mixed powder；
In the mixed powder, nano-sized iron oxide is 47.5 with the mass ratio of step (3) gained powder granule：52.5；
By 1g Dy2O3Powder body is added in above-mentioned gained mixed powder, and mix homogeneously in agate mortar obtains mixture Material；The Dy2O3The quality of powder body for mixed powder quality 5%；
(5) granulating and forming：Step (4) gained mixed material is loaded in mould, under the pressure of 10MPa, single shaft is pressed into Type, then under 180MPa isostatic cool pressings, pressurize 300s obtains green compact；
(6) pyrolysis/sintering：Step (5) gained green compact are loaded in tube furnace, in N2Under atmosphere protection, at 1100 DEG C Temperature is pyrolyzed 4h, 5 DEG C/min of heating rate, obtains final product SiCN (Fe) precursor ceramic of rare earth doped oxide.
Embodiment 3
A kind of method that presoma conversion method prepares SiCN (Fe) precursor ceramic of rare earth doped oxide, including step As follows：
(1) batch mixing：In N2Under atmosphere, polysilazane 9.6g, α-methacrylic acid 2g, cumyl peroxide is weighed 0.4g, adds in reaction bulb, stirs 1h, obtain single transparent mixed solution in constant temperature blender with magnetic force；
Polysilazane in the mixed solution：The mass ratio of cumyl peroxide is 96：4, the α-methacrylic acid Addition be the 20% of polysilazane and cumyl peroxide gross mass；
(2) crosslinking curing：Step (1) gained mixed solution is heated in vacuum tube furnace and is allowed to crosslinking curing, from room Temperature is warming up to 400 DEG C of solidification 4h, and temperature rate is 3 DEG C/min；
(3) ball milling is crushed：The material that step (2) crosslinking curing is obtained is taken, precomminution in agate mortar, then in vibration Ball milling is crushed in ball mill, 100 mesh sieves is crossed, is obtained powder granule；
(4) batch mixing：Take the powder granule 10.5g of step (3) gained, add alpha-iron oxide nano-powder 9.5g, mix homogeneously, Obtain mixed powder；
In the mixed powder, nano-sized iron oxide is 47.5 with the mass ratio of step (3) gained powder granule：52.5；
By 1g Sm2O3Powder body is added in above-mentioned gained mixed powder, and mix homogeneously in agate mortar obtains mixture Material；The Sm2O3The quality of powder body for mixed powder quality 5%；
(5) granulating and forming：Step (4) gained mixed material is loaded in mould, under the pressure of 10MPa, single shaft is pressed into Type, then under 180MPa isostatic cool pressings, pressurize 300s obtains green compact；
(6) pyrolysis/sintering：Step (5) gained green compact are loaded in tube furnace, in N2Under atmosphere protection, at 1300 DEG C Temperature is pyrolyzed 4h, 3 DEG C/min of heating rate, obtains final product SiCN (Fe) precursor ceramic of rare earth doped oxide.
Embodiment 4
A kind of method that presoma conversion method prepares SiCN (Fe) precursor ceramic of rare earth doped oxide, including step As follows：
(1) batch mixing：In N2Under atmosphere, polysilazane 9.6g, α-methacrylic acid 2g, cumyl peroxide is weighed 0.4g, adds in reaction bulb, stirs 1h, obtain single transparent mixed solution in constant temperature blender with magnetic force；
Polysilazane in the mixed solution：Cumyl peroxide obtains mass ratio for 96：4, the α-methacrylic acid Addition be the 20% of polysilazane and cumyl peroxide gross mass；
(2) crosslinking curing：Step (1) gained mixed solution is heated in vacuum tube furnace and is allowed to crosslinking curing, from room Temperature is warming up to 600 DEG C of solidification 4h, and temperature rate is 5 DEG C/min；
(3) ball milling is crushed：The material that step (2) crosslinking curing is obtained is taken, precomminution in agate mortar, then in vibration Ball milling is crushed in ball mill, 100 mesh sieves is crossed, is obtained powder granule；
(4) batch mixing：Step (3) gained powder granule 10.5g is taken, adds alpha-iron oxide nano-powder 9.5g, mix homogeneously to obtain Arrive mixed powder；
In the mixed powder, nano-sized iron oxide is 47.5 with the mass ratio of step (3) gained powder granule：52.5；
By 1g Y2O3Powder body is added in above-mentioned gained mixed powder, and mix homogeneously in agate mortar obtains mixed material； The Y2O3The quality of powder body for mixed powder quality 5%；
(5) granulating and forming：Step (4) gained mixed material is loaded in mould, under the pressure of 10MPa, single shaft is pressed into Type, then under 180MPa isostatic cool pressings, pressurize 300s obtains green compact；
(6) pyrolysis/sintering：Step (5) gained green compact are loaded in tube furnace, in N2Under atmosphere protection, at 1300 DEG C Temperature is pyrolyzed 4h, 5 DEG C/min of heating rate, obtains final product SiCN (Fe) precursor ceramic of rare earth doped oxide.
Embodiment 5
A kind of method that presoma conversion method prepares SiCN (Fe) precursor ceramic of rare earth doped oxide, including step As follows：
(1) batch mixing：In N2Under atmosphere, polysilazane 9.7g, α-methacrylic acid 2g, cumyl peroxide is weighed 0.3g, adds in reaction bulb, stirs 1h, obtain single transparent mixed solution in constant temperature blender with magnetic force；
Polysilazane in the mixed solution：The mass ratio 97 of cumyl peroxide：3, the α-methacrylic acid Addition is the 20% of polysilazane and cumyl peroxide gross mass；
(2) crosslinking curing：Step (1) gained mixed solution is heated in vacuum tube furnace and is allowed to crosslinking curing, from room Temperature is warming up to 400 DEG C of solidification 4h, and temperature rate is 5 DEG C/min；
(3) ball milling is crushed：The material that step (2) crosslinking curing is obtained is taken, precomminution in agate mortar, then in vibration Ball milling is crushed in ball mill, 100 mesh sieves is crossed, is obtained powder granule；
(4) batch mixing：Step (3) gained powder granule 10.5g is taken, adds alpha-iron oxide nano-powder 9.5g, mix homogeneously to obtain Arrive mixed powder；
In the mixed powder, nano-sized iron oxide is 47.5 with the mass ratio of step (3) gained powder granule：52.5；
By 1g Gd2O3Powder body is added in above-mentioned gained mixed powder, and mix homogeneously in agate mortar obtains mixture Material；The Gd2O3The quality of powder body for mixed powder quality 5%；
(5) granulating and forming：Step (4) gained mixed material is loaded in mould, under the pressure of 10MPa, single shaft is pressed into Type, then under 180MPa isostatic cool pressings, pressurize 300s obtains green compact；
(6) pyrolysis/sintering：Step (5) gained green compact are loaded in tube furnace, in N2Under atmosphere protection, at 1400 DEG C Temperature is pyrolyzed 4h, 3 DEG C/min of heating rate, obtains final product SiCN (Fe) precursor ceramic of rare earth doped oxide.
Embodiment 6
A kind of method that presoma conversion method prepares SiCN (Fe) precursor ceramic of rare earth doped oxide, including step As follows：
(1) batch mixing：In N2Under atmosphere, polysilazane 9.8g, α-methacrylic acid 2g, cumyl peroxide is weighed 0.2g, adds in reaction bulb, stirs 1h, obtain single transparent mixed solution in constant temperature blender with magnetic force；
Polysilazane in the mixed solution：The mass ratio of cumyl peroxide is 98：2, the α-methacrylic acid Addition be the 20% of polysilazane and cumyl peroxide gross mass；
(2) crosslinking curing：Step (1) gained mixed solution is heated in vacuum tube furnace and is allowed to crosslinking curing, from room Temperature is warming up to 500 DEG C of solidification 2h, and temperature rate is 4 DEG C/min；
(3) ball milling is crushed：The material that step (2) crosslinking curing is obtained is taken, precomminution in agate mortar, then in vibration Ball milling is crushed in ball mill, 100 mesh sieves is crossed, is obtained powder granule；
(4) batch mixing：The powder granule 10g of step (3) gained is taken, adds alpha-iron oxide nano-powder 10g, mix homogeneously to obtain Arrive mixed powder；
In the mixed powder, nano-sized iron oxide is 1 with the mass ratio of step (3) gained powder granule：1；
By 0.4g Eu2O3Powder body is added in the mixed powder of above-mentioned gained, and mix homogeneously in agate mortar is mixed Material；The Eu2O3The quality of powder body for mixed powder quality 2%；
(5) granulating and forming：Step (4) gained mixed material is loaded in mould, under the pressure of 10MPa, single shaft is pressed into Type, then under 180MPa isostatic cool pressings, pressurize 300s obtains green compact；
(6) pyrolysis/sintering：Step (5) gained green compact are loaded in tube furnace, in N2Under atmosphere protection, at 1000 DEG C Temperature is pyrolyzed 4h, 3 DEG C/min of heating rate, obtains final product SiCN (Fe) precursor ceramic of rare earth doped oxide.
Embodiment 7
A kind of method that presoma conversion method prepares SiCN (Fe) precursor ceramic of rare earth doped oxide, including step As follows：
(1) batch mixing：In N2Under atmosphere, polysilazane 9.8g, α-methacrylic acid 2g, cumyl peroxide is weighed 0.2g, adds in reaction bulb, stirs 1h, obtain single transparent mixed solution in constant temperature blender with magnetic force；
Polysilazane in the mixed solution：The mass ratio of cumyl peroxide is 98：2, the α-methacrylic acid Addition be the 20% of polysilazane and cumyl peroxide gross mass；
(2) crosslinking curing：Step (1) gained mixed solution is heated in vacuum tube furnace and is allowed to crosslinking curing, from room Temperature is warming up to 500 DEG C of solidification 3h, and temperature rate is 4 DEG C/min；
(3) ball milling is crushed：The material that step (2) crosslinking curing is obtained is taken, precomminution in agate mortar, then in vibration Ball milling is crushed in ball mill, 100 mesh sieves is crossed, is obtained powder granule；
(4) batch mixing：Take the powder granule 9.5g of step (3) gained, add alpha-iron oxide nano-powder 10.5g, mix homogeneously, Obtain mixed powder；
In the mixed powder, nano-sized iron oxide is 52.5 with the mass ratio of step (3) gained powder granule：47.5；
By 8g Eu2O3Powder body is added in the mixed powder of above-mentioned gained, and mix homogeneously in agate mortar obtains mixture Material；The Eu2O3The quality of powder body for mixed powder quality 40%；
(5) granulating and forming：Step (4) gained mixed material is loaded in mould, under the pressure of 10MPa, single shaft is pressed into Type, then under 180MPa isostatic cool pressings, pressurize 300s obtains green compact；
(6) pyrolysis/sintering：Step (5) gained green compact are loaded in tube furnace, in N2Under atmosphere protection, at 1000 DEG C Temperature is pyrolyzed 2h, 3 DEG C/min of heating rate, obtains final product SiCN (Fe) precursor ceramic of rare earth doped oxide.
Embodiment 8
A kind of method that presoma conversion method prepares SiCN (Fe) precursor ceramic of rare earth doped oxide, including step As follows：
(1) batch mixing：In N2Under atmosphere, polysilazane 9.8g, α-methacrylic acid 1g, cumyl peroxide is weighed 0.2g, adds in reaction bulb, stirs 1h, obtain single transparent mixed solution in constant temperature blender with magnetic force；
Polysilazane in the mixed solution：The mass ratio of cumyl peroxide is 98：2, the α-methacrylic acid Addition be the 10% of polysilazane and cumyl peroxide gross mass；
(2) crosslinking curing：Step (1) gained mixed solution is heated in vacuum tube furnace and is allowed to crosslinking curing, from room Temperature is warming up to 500 DEG C of solidification 3h, and temperature rate is 4 DEG C/min；
(3) ball milling is crushed：The material that step (2) crosslinking curing is obtained is taken, precomminution in agate mortar, then in vibration Ball milling is crushed in ball mill, 100 mesh sieves is crossed, is obtained powder granule；
(4) batch mixing：Take the powder granule 9.5g of step (3) gained, add alpha-iron oxide nano-powder 10.5g, mix homogeneously, Obtain mixed powder；
In the mixed powder, nano-sized iron oxide is 52.5 with the mass ratio of step (3) gained powder granule：47.5；
By 2g Eu2O3Powder body is added in the mixed powder of above-mentioned gained, and mix homogeneously in agate mortar obtains mixture Material；The Eu2O3The quality of powder body for mixed powder quality 10%；
(5) granulating and forming：Step (4) gained mixed material is loaded in mould, under the pressure of 10MPa, single shaft is pressed into Type, then under 180MPa isostatic cool pressings, pressurize 300s obtains green compact；
(6) pyrolysis/sintering：Step (5) gained green compact are loaded in tube furnace, in N2Under atmosphere protection, at 1000 DEG C Temperature is pyrolyzed 4h, 3 DEG C/min of heating rate, obtains final product SiCN (Fe) precursor ceramic of rare earth doped oxide.
Embodiment 9
A kind of method that presoma conversion method prepares SiCN (Fe) precursor ceramic of rare earth doped oxide, including step As follows：
(1) batch mixing：In N2Under atmosphere, polysilazane 9.8g, α-methacrylic acid 1.5g, cumyl peroxide is weighed 0.2g, adds in reaction bulb, stirs 1h, obtain single transparent mixed solution in constant temperature blender with magnetic force；
Polysilazane in the mixed solution：The mass ratio of cumyl peroxide is 98：2, the α-methacrylic acid Addition be the 15% of polysilazane and cumyl peroxide gross mass；
(2) crosslinking curing：Step (1) gained mixed solution is heated in vacuum tube furnace and is allowed to crosslinking curing, from room Temperature is warming up to 500 DEG C of solidification 3h, and temperature rate is 4 DEG C/min；
(3) ball milling is crushed：The material that step (2) crosslinking curing is obtained is taken, precomminution in agate mortar, then in vibration Ball milling is crushed in ball mill, 100 mesh sieves is crossed, is obtained powder granule；
(4) batch mixing：Take the powder granule 9.5g of step (3) gained, add alpha-iron oxide nano-powder 10.5g, mix homogeneously, Obtain mixed powder；
In the mixed powder, nano-sized iron oxide is 52.5 with the mass ratio of step (3) gained powder granule：47.5；
By 6g Eu2O3Powder body is added in the mixed powder of above-mentioned gained, and mix homogeneously in agate mortar obtains mixture Material；The Eu2O3The quality of powder body for mixed powder quality 30%；
(5) granulating and forming：Step (4) gained mixed material is loaded in mould, under the pressure of 10MPa, single shaft is pressed into Type, then under 180MPa isostatic cool pressings, pressurize 300s obtains green compact；
(6) pyrolysis/sintering：Step (5) gained green compact are loaded in tube furnace, in N2Under atmosphere protection, at 1000 DEG C Temperature is pyrolyzed 3h, 3 DEG C/min of heating rate, obtains final product SiCN (Fe) precursor ceramic of rare earth doped oxide.
Test example 1
SiCN (Fe) precursor ceramic of the rare earth doped oxide that embodiment 1-9 is prepared enters line frequency-reflection Rate R change curve Comparative map is tested, as shown in Fig. 5,6,7.In figure, numeral 1,2,3,4,5,6,7,8,9 is corresponding enforcement respectively The frequency of SiCN (Fe) precursor ceramic of the rare earth doped oxide prepared by example 1,2,3,4,5,6,7,8,9-reflectance R becomes Change curve.
SiCN (Fe) precursor ceramic of the rare earth doped oxide that embodiment 1-9 is prepared enters line frequency-electromagnetism Attenuation quotient a change curves Comparative map is tested, as shown in Figure 8,9, 10.In figure, numeral 1,2,3,4,5,6,7,8,9 is respectively The frequency of SiCN (Fe) precursor ceramic of the rare earth doped oxide prepared by corresponding embodiment 1,2,3,4,5,6,7,8,9- Electromagnetic attenuation coefficient a change curves.
Contrasted from Fig. 5-10, with the increase of frequency, reflectance is in reduction trend, and electromagnetic attenuation coefficient is in increase Trend, i.e. sample electromagnetic wave absorption performance increase with the increase of frequency, and mix Eu2O3Sample variation amplitude maximum, In the range of 16-17GHz, reflectance has minima, electromagnetic attenuation coefficient to reach maximum, it follows that doping Eu2O3Sample inhale ripple Best performance.
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-described embodiment, there can also be other deformations.Those skilled in the art directly derive from the disclosure of invention or All deformations of amplification, are considered as protection scope of the present invention indirectly.

Claims (10)

1. a kind of method that presoma conversion method prepares SiCN (Fe) precursor ceramic of rare earth doped oxide, including step such as Under：
(1) batch mixing：Under an inert atmosphere, polysilazane, α-methacrylic acid and cumyl peroxide are mixed 1-2h, Obtain mixed solution；
The polysilazane：The mass ratio of cumyl peroxide is 96-98：2-4；The addition of the α-methacrylic acid is Polysilazane and the 10%-20% of cumyl peroxide gross mass；
(2) crosslinking curing：By step (1) gained mixed solution at 400 DEG C -600 DEG C, under vacuum condition, solidify 2-4h；
(3) ball milling is crushed：Material that step (2) crosslinking curing is obtained is pre-milled, crush ball milling, sieve, and obtains powder body Grain；
(4) batch mixing：Alpha-iron oxide nano-powder, mix homogeneously is added to obtain mixed powder in the powder granule obtained to step (3)； RE oxide powder is subsequently adding, mix homogeneously obtains mixed material；
(5) granulating and forming：Will be compressing for step (4) gained mixed material, isostatic cool pressing, pressurize obtain green compact；
(6) pyrolysis/sintering：By step (5) gained green compact under inert gas shielding, sinter in 1000 DEG C -1400 DEG C of temperature 2-4h, obtains final product SiCN (Fe) precursor ceramic of rare earth doped oxide.
2. presoma conversion method according to claim 1 prepares SiCN (Fe) precursor ceramic of rare earth doped oxide Method, it is characterised in that polysilazane is HTT1800 in step (1).
3. presoma conversion method according to claim 1 prepares SiCN (Fe) precursor ceramic of rare earth doped oxide Method, it is characterised in that polysilazane in step (1)：The mass ratio of cumyl peroxide is 98：2.
4. presoma conversion method according to claim 1 prepares SiCN (Fe) precursor ceramic of rare earth doped oxide Method, it is characterised in that inert atmosphere is nitrogen, argon or helium atmosphere in step (1).
5. presoma conversion method according to claim 1 prepares SiCN (Fe) precursor ceramic of rare earth doped oxide Method, it is characterised in that heating rate is 2-5 DEG C/min in step (2)；Solidification temperature 500-600 DEG C, hardening time 3- 4h；
Preferably, heating rate is 3-4 DEG C/min.
6. presoma conversion method according to claim 1 prepares SiCN (Fe) precursor ceramic of rare earth doped oxide Method, it is characterised in that nano-sized iron oxide is 40-60 with the mass ratio of step (3) gained powder granule in step (4)： 40-60.
7. presoma conversion method according to claim 1 prepares SiCN (Fe) precursor ceramic of rare earth doped oxide Method, it is characterised in that 2%-40% of the addition of step (4) middle rare earth for mixed powder quality；
Preferably, 10%-30% of the addition of rare earth oxide for mixed powder quality；
It is further preferred that the addition of rare earth oxide is the 5% of mixed powder quality.
8. presoma conversion method according to claim 1 prepares SiCN (Fe) precursor ceramic of rare earth doped oxide Method, it is characterised in that step (4) middle rare earth is Dy2O3、Eu2O3、Sm2O3、Y2O3Or Gd2O3；
Preferably, the rare earth oxide is Eu2O3.
9. presoma conversion method according to claim 1 prepares SiCN (Fe) precursor ceramic of rare earth doped oxide Method, it is characterised in that compressing under the pressure of 10MPa in step (5)；
Preferably, in step (5), isostatic cool pressing is carried out under 180MPa, pressurize 300s.
10. presoma conversion method according to claim 1 prepares SiCN (Fe) precursor ceramic of rare earth doped oxide Method, it is characterised in that in step (6) heating rate be 3-5 DEG C/min.
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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
WO2019061485A1 (en) * 2017-09-29 2019-04-04 山东大学 Method for preparing europium oxide-doped iron-containing silicon-carbon-nitrogen precursor ceramic
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CN110576498B (en) * 2018-06-08 2021-08-31 中国科学院沈阳自动化研究所 Additive manufacturing device and process for ceramic precursor material
CN110451986A (en) * 2019-09-09 2019-11-15 中国人民解放军国防科技大学 Photocuring 3D printing SiCN ceramic precursor material and application thereof
CN110451986B (en) * 2019-09-09 2021-12-10 中国人民解放军国防科技大学 Photocuring 3D printing SiCN ceramic precursor material and application thereof
CN113896543A (en) * 2021-10-11 2022-01-07 西北工业大学 Wave-absorbing silicon-carbon-nitrogen ceramic with layered structure and preparation method thereof
CN113896543B (en) * 2021-10-11 2023-03-14 西北工业大学 Wave-absorbing silicon-carbon-nitrogen ceramic with layered structure and preparation method thereof
CN116409999A (en) * 2023-03-22 2023-07-11 南京信息工程大学 S-band silicon-carbon-nitrogen ceramic wave-absorbing material 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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