CN102351541A - In-situ preparation method for Y4Si2O7N2-BN ceramic base composite materials - Google Patents
In-situ preparation method for Y4Si2O7N2-BN ceramic base composite materials Download PDFInfo
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Abstract
The invention relates to the field of ceramic base composite materials, in particular to an in-situ preparation method for Y4Si2O7N2-BN ceramic base composite materials. The composite materials consist of two phases: Y4Si2O7N2 and BN, wherein the content of the BN in the composite materials is 5 to 95 percent through being metered in percentage by volume, and the balance is the Y4Si2O7N2. Yttrium oxide powder, silicon oxide powder, silicon nitride powder and BN powder are used as raw materials, material powder carries out ball milling for 1 to 24 hours, the materials are charged into a graphite mold after being baked and sieved, the cold pressing is carried out at 10 to 15MPa, then, the temperature is raised to 1500 to 1700 DEG C at a temperature rise velocity of 5 to 40 DEG C/min in a hot pressing furnace by using nitrogen gas as protection atmosphere, the temperature is preserved for 0.5 to 1 hour, then, the temperature is raised to 1800 to 2100 DEG C at a temperature rise velocity of 5 to 40 DEG C/min, the temperature is preserved for 1 to 3 hours, and the hot pressing pressure is 10 to 40 MPa. The Y4Si2O7N2-BN ceramic base composite materials with high purity, good density, high intensity and low heat conductivity can be sintered through hot pressing in a short time.
Description
Technical field
The present invention relates to the ceramic matric composite field, be specially a kind of yttrium silica nitrogen-boron nitride (Y
4Si
2O
7N
2-BN) the in-situ preparation method of ceramic matric composite.
Background technology
Y
4Si
2O
7N
2It is a kind of novel quaternary lower thermal conductivity stupalith.It has plurality of advantages aspect thermal property, it has lower thermal conductivity (room temperature thermal conductivity 1.8-2.0Wm
-1K
-1, 1000 ℃ of elevated temperature heat conductance 1.4-1.6Wm
-1K
-1), lower thermal expansivity (4-6 * 10
-6K
-1), good high temperature resistant, antioxidant property, lower density (4.83g/cm
3) and modulus (Young's modulus 185GPa), (flexural strength 157 ± 7MPa), (Vickers' hardness 10.3 ± 0.3GPa) etc. all have potential application foreground widely at high-technology fields such as Aeronautics and Astronautics, Iron And Steel Industry to higher hardness to medium tenacity.Although Y
4Si
2O
7N
2Have excellent thermal property, but its relatively poor workability, heat-shock resistance, and big limitations such as intrinsic fragility its application.At Y
4Si
2O
7N
2Add BN in the matrix and prepare matrix material and can improve above-mentioned unfavorable performance, yet with Y
4Si
2O
7N
2Powder and BN powder are that this matrix material of feedstock production exists density and mechanical property to remain further to be improved, and thermal conductivity also remains further to be reduced.To these problems, the present invention develops a kind of employing h-BN powder, Y
2O
3Powder, SiO
2Powder and Si
3N
4Powder prepares Y for the raw material reaction in
4Si
2O
7N
2The method of-BN matrix material.
Summary of the invention:
The object of the invention is to provide the method for the yttrium silica nitrogen-boron nitride ceramic matric composite that a kind of in-situ preparing can be processed, mechanical property is good, thermal conductivity is low; It is lower to solve the matrix material density and the mechanical property that exist in the prior art, and thermal conductivity is than problems such as height.
Technical scheme of the present invention is:
A kind of in-situ preparation method of yttrium silica nitrogen-boron nitride ceramic matric composite comprises the steps:
1) raw material powder is formed and composition range:
With hexagonal boron nitride (h-BN) powder, Y
2O
3Powder, SiO
2Powder and Si
3N
4Powder is a raw material, h-BN powder, Y
2O
3Powder, SiO
2Powder and Si
3N
4The mol ratio of powder is (4.5～28.4): 4: 1: 1;
2) preparation technology:
Raw material process ball milling 1～24 hour; Pack in the graphite jig; Cold pressing with the pressure of 10～15MPa and to become pie in 1～5 minute; Rise to 1500～1700 ℃ of insulations 0.5～1 hour with the temperature rise rate of 5～40 ℃/min in as the hot pressing furnace of protective atmosphere being connected with nitrogen; Then the temperature rise rate with 5～40 ℃/min rises to 1800～2100 ℃ of insulations 1～3 hour, and hot pressing pressure is 20～40MPa.It is free from foreign meter by Y to utilize above-mentioned technology finally to obtain
4Si
2O
7N
2With the matrix material of h-BN two phase composites, the volume content of boron nitride is 5～95% (being preferably 10～30%), and h-BN second phase size (is preferably 0.5-5 μ m) in the matrix material below 5 μ m, with isolated island shape even dispersion be distributed in successive Y
4Si
2O
7N
2In the middle of the matrix.
Among the present invention, Y
2O
3The granularity of powder is 100～400 orders, SiO
2The granularity of powder is 100～400 orders, Si
3N
4The granularity of powder is 100～300 orders, and the granularity of h-BN powder is 100～300 orders.
Among the present invention, ball milling is that silicon nitride ball adds the wet-milling that ethanol carries out routine.
Advantage of the present invention is:
1. the material composition of the present invention's use is common, is respectively h-BN powder, Y
2O
3Powder, SiO
2Powder and Si
3N
4Powder.
2. technology is simple, and cost is low.The present invention obtains the fine and close Y of inclusion-free through a simple step in-situ hot pressing synthetic method at (below 2100 ℃) and short period of time (generally in three hours)
4Si
2O
7N
2-BN ceramic matric composite.
3. higher density, low thermal conductivity and excellent mechanical property.Y of the present invention
4Si
2O
7N
2-BN ceramic matric composite density, flexural strength and fracture toughness property etc. are better than adopting Y
4Si
2O
7N
2The Y of powder and the preparation of h-BN powder sintering
4Si
2O
7N
2-BN ceramic matric composite.And thermal conductivity is lower than employing Y
4Si
2O
7N
2The Y of powder and the preparation of h-BN powder sintering
4Si
2O
7N
2-BN ceramic matric composite.
Description of drawings
Fig. 1 is in-situ preparing Y
4Si
2O
7N
2The XRD figure spectrum of-10vol.%BN matrix material.
Fig. 2 is in-situ preparing Y
4Si
2O
7N
2The thermal conductivity of-20vol.%BN matrix material.
Fig. 3 is in-situ preparing Y
4Si
2O
7N
2Two of-40vol.%BN matrix material the pattern that distributes mutually.
Embodiment
Through instance the present invention is detailed below.
Embodiment 1
With h-BN powder (100 orders, purity: 99wt.%) 4.45g, Y
2O
3Powder (300 orders, purity: 99.5wt.%) 69.83g, SiO
2Powder (200 orders, purity: 99.5wt.%) 4.66g and Si
3N
4(300 orders, purity: 99wt.%) 10.83g pours in the silicon nitride ball milling jar powder, uses silicon nitride ball to add ethanol wet-milling 12 hours, afterwards 50 ℃ of oven dry 48 hours.It is that the inwall of 50mm scribbles in the graphite jig of BN and colds pressing that powder after the oven dry is poured diameter into.Cold pressing after the 5min with the pressure of 12MPa, mould is packed in the hot pressing furnace, under the flowing nitrogen protection; Temperature rise rate with 5 ℃/min is warming up to 1600 ℃, insulation 30min, and the temperature rise rate with 10 ℃/min is warming up to 1800 ℃ afterwards; Hot pressing 60min, hot pressing pressure are 30MPa.The block materials that obtains is Y through X-ray diffraction analysis
4Si
2O
7N
2With BN two mutually, the two volume ratio is 90: 10, does not have other impurity basically.The density of measuring is 4.37g/cm
3, density is 95.53%.Three-point bending strength is 239 ± 23MPa, Vickers' hardness 7.97 ± 0.2GPa.Matrix material XRD figure spectrum as shown in Figure 1.
Embodiment 2
With h-BN powder (100 orders, purity: 99wt.%) 12.68g, Y
2O
3Powder (300 orders, purity: 99.5wt.%) 88.3g, SiO
2Powder (200 orders, purity: 99.5wt.%) 5.89g and Si
3N
4(200 orders, purity: 99wt.%) 13.7g pours in the silicon nitride ball milling jar powder, uses silicon nitride ball to add ethanol wet-milling 24 hours, dries 48 hours for 50 ℃ afterwards.It is that the inwall of 50mm scribbles in the graphite jig of BN and colds pressing that powder after the oven dry is poured diameter into.After colding pressing 3 minutes with the pressure of 15MPa, mould is packed in the hot pressing furnace of graphite heater, under the flowing nitrogen protection; Temperature rise rate with 15 ℃/min is warming up to 1550 ℃, and insulation 40min is warming up to 1900 ℃ afterwards; Hot pressing 50min, hot pressing pressure are 30MPa.The matrix material that obtains is Y through X-ray diffraction analysis
4Si
2O
7N
2With BN two mutually, the two volume ratio is 80: 20, does not have other impurity basically.The density of material of measuring is 4.136g/cm
3, density is 95.80%.Three-point bending strength is 344 ± 13MPa, fracture toughness property 2.15 ± 0.22MPam
1/2, the matrix material thermal conductivity varies with temperature as shown in Figure 2.
Embodiment 3
With h-BN powder (300 orders, purity: 99wt.%) 17.82g, Y
2O
3Powder (400 orders, purity: 99.5wt.%) 46,56g, SiO
2Powder (200 orders, purity: 99.5wt.%) 3.11g and Si
3N
4(300 orders, purity: 99wt.%) 7.22g pours in the silicon nitride ball milling jar powder, uses silicon nitride ball to add ethanol wet-milling 6 hours, dries 48 hours for 50 ℃ afterwards.It is that the inwall of 50mm scribbles in the graphite jig of BN and colds pressing that powder after the oven dry is poured diameter into.After colding pressing 4 minutes with the pressure of 10MPa, mould is packed in the hot pressing furnace of graphite heater, under the flowing nitrogen protection; Temperature rise rate with 30 ℃/min is warming up to 1700 ℃, and insulation 30min is warming up to 2100 ℃ afterwards; Hot pressing 30min, hot pressing pressure are 20MPa.The matrix material that obtains is Y through X-ray diffraction analysis
4Si
2O
7N
2With BN two mutually, the two volume ratio is 60: 40.The density of material of measuring is 3.65g/cm
3, density is 95.84%.Three-point bending strength is 298 ± 32MPa, and the room temperature Young's modulus is 118.81GPa.
As shown in Figure 3, h-BN second phase size (present embodiment is 0.5-5 μ m) below 5 μ m in the matrix material, with isolated island shape even dispersion be distributed in successive Y
4Si
2O
7N
2In the middle of the matrix.
Comparative example 1
With Y
4Si
2O
7N
2(300 orders, purity: 99wt.%) 77.62g, (100 orders, purity: 99wt.%) 9.12g pours in the silicon nitride ball milling jar h-BN powder powder, uses silicon nitride ball to add ethanol wet-milling 24 hours, dries 48 hours for 50 ℃ afterwards.It is that the inwall of 50mm scribbles in the graphite jig of BN and colds pressing that powder after the oven dry is poured diameter into.After colding pressing 3 minutes with the pressure of 15MPa, mould is packed in the hot pressing furnace of graphite heater, under the flowing nitrogen protection, be warming up to 1800 ℃ with the temperature rise rate of 15 ℃/min, hot pressing 60min, hot pressing pressure are 40MPa.The matrix material that obtains is Y through X-ray diffraction analysis
4Si
2O
7N
2With BN two mutually, the two volume ratio is 80: 20, does not have other impurity basically.The density of material of measuring is 4.09g/cm
3, density is 94.74%.Three-point bending strength is 286 ± 12MPa, fracture toughness property 2.04 ± 0.03MPam
1/2
Can find out from comparative example, with Y
4Si
2O
7N
2Powder and BN powder are that this matrix material density and the mechanical property of feedstock production remains further to be improved, and thermal conductivity also remains further to be reduced.Utilize the fracture mechanics of brittle ceramic and the correlation theory of ceramic composite thermal conductivity to analyze, we reach a conclusion: when the h-BN size further reduces, and when distributing more disperse, Y
4Si
2O
7N
2The mechanical property of-BN matrix material is expected to further raising, and thermal conductivity can further reduce.
Can find out that from embodiment the present invention can go out the yttrium silica nitrogen-boron nitride ceramic matric composite that purity height, good compactness, intensity are high, thermal conductivity is low with shorter time and less step hot pressed sintering.
Claims (5)
1. the in-situ preparation method of a yttrium silica nitrogen-boron nitride ceramic matric composite is characterized in that:
1) raw material powder is formed:
With h-BN powder, Y
2O
3Powder, SiO
2Powder and Si
3N
4Powder is a raw material, h-BN powder, Y
2O
3Powder, SiO
2Powder and Si
3N
4The mol ratio of powder is (4.5～28.4): 4: 1: 1;
2) preparation technology:
Raw material process ball milling 1～24 hour; Pack in the graphite jig; Cold pressing with the pressure of 10～15MPa and to become pie in 1～5 minute; Rise to 1500～1700 ℃ of insulations 0.5～1 hour with the temperature rise rate of 5～40 ℃/min in as the hot pressing furnace of protective atmosphere being connected with nitrogen; Then the temperature rise rate with 5～40 ℃/min rises to 1800～2100 ℃ of insulations 1～3 hour, and hot pressing pressure is 10～40MPa.
2. according to the in-situ preparation method of the described yttrium silica of claim 1 nitrogen-boron nitride ceramic matric composite, it is characterized in that Y
2O
3The granularity of powder is 100～400 orders, SiO
2The granularity of powder is 100～400 orders, Si
3N
4The granularity of powder is 100～300 orders, and the granularity of h-BN powder is 100～300 orders.
3. according to the in-situ preparation method of the described yttrium silica of claim 1 nitrogen-boron nitride ceramic matric composite, it is characterized in that the volume content of boron nitride is 5～95%, all the other are Y
4Si
2O
7N
2Phase.
4. according to the in-situ preparation method of the described yttrium silica of claim 1 nitrogen-boron nitride ceramic matric composite, it is characterized in that the volume content of boron nitride is preferably 10～30%, all the other are Y
4Si
2O
7N
2Phase.
5. according to the in-situ preparation method of the described yttrium silica of claim 1 nitrogen-boron nitride ceramic matric composite, it is characterized in that, in the matrix material h-BN second phase size below 5 μ m, with isolated island shape even dispersion be distributed in successive Y
4Si
2O
7N
2In the middle of the matrix.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103936424A (en) * | 2014-04-15 | 2014-07-23 | 中国科学院金属研究所 | Hexagonal boron nitride-yttrium silicon oxide composite material and preparation method thereof |
| CN106278283A (en) * | 2016-08-04 | 2017-01-04 | 长兴鑫宇耐火材料有限公司 | A kind of step sintering prepares the method for boron nitride ceramic material |
| CN108002841A (en) * | 2017-03-30 | 2018-05-08 | 中国科学院金属研究所 | Hexagonal boron nitride-ytterbium silica nitrogen ceramic matric composite and its in-situ preparation method |
| CN114195538A (en) * | 2021-12-24 | 2022-03-18 | 中国科学院上海硅酸盐研究所 | Preparation method of compact hexagonal boron nitride ceramic material |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101050115A (en) * | 2007-03-09 | 2007-10-10 | 西南科技大学 | Ceramics of containing powder body of cubic silicon nitride, and preparation method |
| CN101555156A (en) * | 2009-05-15 | 2009-10-14 | 山东大学 | Boron nitride crystal whisker/silicon nitride ceramic composite material and preparation method thereof |
-
2011
- 2011-06-29 CN CN 201110180000 patent/CN102351541B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101050115A (en) * | 2007-03-09 | 2007-10-10 | 西南科技大学 | Ceramics of containing powder body of cubic silicon nitride, and preparation method |
| CN101555156A (en) * | 2009-05-15 | 2009-10-14 | 山东大学 | Boron nitride crystal whisker/silicon nitride ceramic composite material and preparation method thereof |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103936424A (en) * | 2014-04-15 | 2014-07-23 | 中国科学院金属研究所 | Hexagonal boron nitride-yttrium silicon oxide composite material and preparation method thereof |
| CN103936424B (en) * | 2014-04-15 | 2015-07-08 | 中国科学院金属研究所 | Hexagonal boron nitride-yttrium silicon oxide composite material and preparation method thereof |
| CN106278283A (en) * | 2016-08-04 | 2017-01-04 | 长兴鑫宇耐火材料有限公司 | A kind of step sintering prepares the method for boron nitride ceramic material |
| CN108002841A (en) * | 2017-03-30 | 2018-05-08 | 中国科学院金属研究所 | Hexagonal boron nitride-ytterbium silica nitrogen ceramic matric composite and its in-situ preparation method |
| CN108002841B (en) * | 2017-03-30 | 2021-01-08 | 中国科学院金属研究所 | Hexagonal boron nitride-ytterbium silicon oxynitride ceramic matrix composite material and in-situ preparation method thereof |
| CN114195538A (en) * | 2021-12-24 | 2022-03-18 | 中国科学院上海硅酸盐研究所 | Preparation method of compact hexagonal boron nitride ceramic material |
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