CN104817325A - Preparation method of reactive sintered boron carbide-silicon carbide composite ceramic material - Google Patents
Preparation method of reactive sintered boron carbide-silicon carbide composite ceramic material Download PDFInfo
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- CN104817325A CN104817325A CN201510256908.3A CN201510256908A CN104817325A CN 104817325 A CN104817325 A CN 104817325A CN 201510256908 A CN201510256908 A CN 201510256908A CN 104817325 A CN104817325 A CN 104817325A
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Abstract
The invention relates to a preparation method of a reactive sintered boron carbide-silicon carbide composite ceramic material. The preparation method comprises the following steps: (1) mixing: ball milling raw materials (80-90wt% of boron carbide, 5-18wt% of carbon dust and 1-5wt% of a sintering aid) in a ball milling tank; (2) molding: putting the mixture obtained in the step (1) in a mold and performing dry pressing molding to obtain a boron carbide ceramic biscuit; (3) reactive sintering: putting the boron carbide ceramic biscuit obtained in the step (2) in a reactive sintering furnace; sintering at a high temperature in vacuum for infiltrating and melting a metal silicon wafer to obtain the reactive sintered boron carbide-silicon carbide composite ceramic material. The method disclosed by the invention, raw materials and proportion are scientific and reasonable; the production method is safe and low in cost; the prepared boron carbide-silicon carbide composite ceramic material is capable of meeting the thermal neutron shielding performance requirement for waste in the nuclear industry.
Description
Technical field
The present invention relates to a kind of preparation method of stupalith, particularly relate to a kind of preparation method of composite ceramic material, belong to material science.
Background technology
Norbide has high-melting-point, high rigidity, low density and the advantage such as good thermostability and solidity to corrosion, but because boron carbide ceramics exists poor toughness and the shortcomings such as hard-to-sinter densification, some special engineering application requiring can not be met, and toughening effect can be reached by adding second-phase, thus meet engineer applied demand, and thyrite is with the hot strength of its uniqueness, stable chemical, superhard wear, thermal shock resistance, and the excellent properties such as the coefficient of expansion is low, therefore the toughness of norbide is improved by adding silicon carbide, and its original physical and mechanical properties can be kept, become a kind of selection well.
Sintering process conventional at present has pressureless sintering, hot pressed sintering and reaction sintering etc., and wherein the cost of hot pressed sintering is higher, and harsh to dimensional requirement, is unfavorable for producing in enormous quantities; Pressureless sintering needs higher sintering temperature, and sintering is difficulty comparatively, and cost is high, after sintering, size changes, thus its use is subject to a definite limitation, but reaction sintering has that technique is simple, cost is low, sintering time ask the advantages such as short, sintering temperature is low, net-shape-sinter, compensate for the deficiency of hot pressed sintering to dimensional requirement harshness, simultaneously, reduce sintering temperature, shorten sintering time, and then reduce cost, therefore reaction sintering tool has great advantage, and has broad prospect of application.Norbide/silicon carbide composite ceramic materials is the ceramic of compact sintered compact that application molten silicon infiltration carbon containing boron carbide ceramics biscuit obtains.And because the method has, sintering temperature is low, sintering time is short, base substrate Shou Shrink leads little (< 3%), is easy to prepare the features such as big-size complicated shape component, the most applicable suitability for industrialized production.
Summary of the invention
The present invention is directed to the deficiency of existing boron carbide ceramics material in application aspect, the preparation method of a kind of reaction sintering norbide-silicon carbide composite ceramic materials is provided.
The technical scheme that the present invention solves the problems of the technologies described above is as follows:
A preparation method for reaction sintering norbide-silicon carbide composite ceramic materials, is characterized in that, comprise the steps:
(1) batch mixing: be the norbide of 80 ~ 90% respectively using weight percent, the carbon dust of 5 ~ 18%, the sintering aid of 1 ~ 5% put into ball grinder ball milling 5 ~ 10 hours as raw material;
(2) shaping: gained compound in step (1) is placed in mould, dry-pressing formed through 80 ~ 120M Pa, obtain boron carbide ceramics biscuit;
(3) reaction sintering: gained boron carbide ceramics biscuit in step (2) is put into reaction sintering stove, the silicon chip adding 1 ~ 2 weight part in every 100 weight part biscuit of ceramics carries out vacuum siliconising reaction sintering, obtains reaction sintering norbide-silicon carbide composite ceramic materials.
The invention has the beneficial effects as follows: raw material and the proportioning of method employing of the present invention are scientific and reasonable, and safe production process, cost are low, and made norbide-silicon carbide composite ceramic materials can meet the thermal neutron shielding properties requirement of the weary waste material of nuclear industry.
On the basis of technique scheme, the present invention can also do following improvement.
Further, sintering aid described in step (1) is the mixture of boron or boron and norbide.
Further, described in step (3), vacuum sintering process is: low temperature 500 ~ 900 DEG C, keeps 3 ~ 5 hours, middle temperature 900 ~ 1450 DEG C, keeps 4 ~ 6 hours, high temperature 1450 ~ 1700 DEG C, keeps 1 ~ 3 hour, heat-up rate 10 ~ 20 DEG C/min.
Accompanying drawing explanation
Fig. 1 is the XRD spectra of the norbide-silicon carbide composite ceramic materials of gained of the present invention;
Fig. 2 is the SEM figure of the norbide-silicon carbide composite ceramic materials of the embodiment of the present invention 1 gained;
In Fig. 1, (1) represents embodiment 1; (2) embodiment 2 is represented; (3) embodiment 3 is represented;
Embodiment
Be described principle of the present invention and feature below in conjunction with example, example, only for explaining the present invention, is not intended to limit scope of the present invention.
Embodiment 1:
By 800g norbide, 180g carbon dust, 20g boron puts into ball grinder ball milling 5 hours as raw material, gained compound is placed in mould, dry-pressing formed through 100MPa, obtain boron carbide ceramics biscuit, boron carbide ceramics biscuit is put into reaction sintering stove, vacuum high-temperature sintering process is: heat-up rate: 10 DEG C/min, low temperature 700 DEG C, keep 5 hours, middle temperature: 1200 DEG C, keep 4 hours, high temperature 1550 DEG C, keep 2 hours, lower the temperature with stove afterwards, obtain reaction sintering norbide-silicon carbide composite ceramic materials, in Fig. 1, a bottom curve is its XRD spectra.
Embodiment 2:
900g norbide, 50g carbon dust, 50g boron are put into ball grinder ball milling 10 hours as raw material, gained compound is placed in mould, dry-pressing formed through 120MPa, obtain boron carbide ceramics biscuit, boron carbide ceramics biscuit is put into reaction sintering stove, vacuum high-temperature sintering process is: heat-up rate: 15 DEG C/min, low temperature 500 DEG C, keeps 4 hours, middle temperature: 1450 DEG C, keep 5 hours, high temperature 1700 DEG C, keeps 1 hour, lowers the temperature afterwards with stove, obtain reaction sintering norbide-silicon carbide composite ceramic materials, in the middle of in Fig. 1, a curve is its XRD spectra.
Embodiment 3:
By 850g norbide, 110g carbon dust, 40g boron puts into ball grinder ball milling 7 hours as raw material, gained compound is placed in mould, dry-pressing formed through 80MPa, obtain boron carbide ceramics biscuit, boron carbide ceramics biscuit is put into reaction sintering stove, vacuum high-temperature sintering process is: heat-up rate: 20 DEG C/min, low temperature 900 DEG C, keep 3 hours, middle temperature: 1200 DEG C, keep 4 hours, high temperature 1450 DEG C, keep 2 hours, lower the temperature with stove afterwards, obtain reaction sintering norbide-silicon carbide composite ceramic materials, in Fig. 1, topmost a curve is its XRD spectra.
Table 1: gained composite property test result in embodiment 1-3
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., within the protection domain that all should be included in invention.
Claims (3)
1. a preparation method for reaction sintering norbide-silicon carbide composite ceramic materials, is characterized in that, comprise the steps:
(1) batch mixing: be the norbide of 80 ~ 90% respectively using weight percent, the carbon dust of 5 ~ 18%, the sintering aid of 1 ~ 5% put into ball grinder ball milling 5 ~ 10 hours as raw material;
(2) shaping: gained compound in step (1) is placed in mould, dry-pressing formed through 80 ~ 120MPa, obtain boron carbide ceramics biscuit;
(3) reaction sintering: gained boron carbide ceramics biscuit in step (2) is put into reaction sintering stove, the silicon chip adding 1 ~ 2 weight part in every 100 weight part biscuit of ceramics carries out vacuum siliconising reaction sintering, obtains reaction sintering norbide-silicon carbide composite ceramic materials.
2. the preparation method of a kind of reaction sintering norbide-silicon carbide composite ceramic materials according to claim 1, is characterized in that, sintering aid described in step (1) is the mixture of boron or boron and norbide.
3. the preparation method of a kind of reaction sintering norbide-silicon carbide composite ceramic materials according to claim 1, it is characterized in that, described in step (3), vacuum sintering process is: low temperature 500 ~ 900 DEG C, keep 3 ~ 5 hours, middle temperature 900 ~ 1450 DEG C, keeps 4 ~ 6 hours, high temperature 1450 ~ 1700 DEG C, keep 1 ~ 3 hour, heat-up rate 10 ~ 20 DEG C/min.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105777130A (en) * | 2016-03-17 | 2016-07-20 | 东北大学 | Gel casing preparation method of reaction-sintered boron carbide ceramic composite material |
| CN106478103A (en) * | 2015-09-01 | 2017-03-08 | 常熟佳合高级陶瓷材料有限公司 | A kind of preparation method of silicon carbide/carbon boron composite ceramic material |
| CN107141004A (en) * | 2017-06-13 | 2017-09-08 | 华中科技大学 | A kind of boron carbide composite material and preparation method thereof |
| CN108658603A (en) * | 2017-12-25 | 2018-10-16 | 成都晋阳科技有限公司 | A kind of preparation method of silicon carbide boron carbide composite material |
| CN108863442A (en) * | 2018-06-13 | 2018-11-23 | 南京航空航天大学 | A kind of neutron shield composite material and preparation method |
| CN109400166A (en) * | 2019-01-12 | 2019-03-01 | 东北大学 | The method of crystalline silicon diamond wire cutting waste material preparation Boron carbide silicon carbide composite ceramic |
| CN111933322A (en) * | 2020-08-13 | 2020-11-13 | 中国核动力研究设计院 | High-temperature-resistant neutron shielding assembly and preparation method thereof |
| CN114621024A (en) * | 2022-03-23 | 2022-06-14 | 山东华屹科创纳米材料有限公司 | High-purity toughened boron carbide foamed ceramic and preparation method thereof |
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2015
- 2015-05-19 CN CN201510256908.3A patent/CN104817325A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106478103A (en) * | 2015-09-01 | 2017-03-08 | 常熟佳合高级陶瓷材料有限公司 | A kind of preparation method of silicon carbide/carbon boron composite ceramic material |
| CN105777130A (en) * | 2016-03-17 | 2016-07-20 | 东北大学 | Gel casing preparation method of reaction-sintered boron carbide ceramic composite material |
| CN107141004A (en) * | 2017-06-13 | 2017-09-08 | 华中科技大学 | A kind of boron carbide composite material and preparation method thereof |
| CN108658603A (en) * | 2017-12-25 | 2018-10-16 | 成都晋阳科技有限公司 | A kind of preparation method of silicon carbide boron carbide composite material |
| CN108863442A (en) * | 2018-06-13 | 2018-11-23 | 南京航空航天大学 | A kind of neutron shield composite material and preparation method |
| CN109400166A (en) * | 2019-01-12 | 2019-03-01 | 东北大学 | The method of crystalline silicon diamond wire cutting waste material preparation Boron carbide silicon carbide composite ceramic |
| CN111933322A (en) * | 2020-08-13 | 2020-11-13 | 中国核动力研究设计院 | High-temperature-resistant neutron shielding assembly and preparation method thereof |
| CN111933322B (en) * | 2020-08-13 | 2022-11-22 | 中国核动力研究设计院 | High-temperature-resistant neutron shielding assembly and preparation method thereof |
| CN114621024A (en) * | 2022-03-23 | 2022-06-14 | 山东华屹科创纳米材料有限公司 | High-purity toughened boron carbide foamed ceramic and preparation method thereof |
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