CN110395988A - A kind of high intensity boron nitride ceramics and preparation method thereof - Google Patents
A kind of high intensity boron nitride ceramics and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of high-intensitive boron nitride ceramics and preparation method thereof, and preparation method is the following steps are included: A) charging: the single particle size nano cubic boron nitride powder of certain mass is weighed, the preformed compact after pre-molding is put into sintering mold by pre-molding；B it) is sintered: the preformed compact in step A) being put into togerther in discharging plasma sintering equipment or hot-press sintering equipment together with sintering mold and is sintered；C it) discharges: taking out mold after temperature in equipment is cooled to room temperature, move back mould and obtain high-intensitive boron nitride ceramics block.The present invention obtains high-intensitive boron nitride ceramics by the nano cubic boron nitride powder of sintering single particle size.
Description
Technical field
The present invention relates to structural ceramics preparation technical field, especially a kind of high-intensitive boron nitride ceramics and its preparation side
Method.
Background technique
The bulk that hexagonal boron nitride (hBN) ceramics are formed generally by sintering hexagonal boron nitride powder is a kind of advanced
Structural ceramics.It has excellent physical characteristic, including high-insulativity, low-k, high heat conductance and excellent heat resistanceheat resistant
Pinking etc., therefore be widely used.But due to its ceramic special layer structure of hexagonal boron nitride, in C axis direction
Binding force is far smaller than the binding force perpendicular to C axis direction, and crystal is mainly grown along board direction, the growth fraction of through-thickness
Relatively slowly, to form flat crystal structure, card bridging structure is formed when this flat crystal structure is sintered, plays mutual branch
The effect of support hinders the contraction of material, so that the hBN ceramic dense degree obtained is lower, adds model moral between layers
Hua Li very weak influence causes the bad mechanical property of the hexagonal boron nitride prepared ceramics, intensity lower, strongly limit its into
The development of one step and application.
Since hexagonal boron nitride ceramics are difficult to be sintered, pure hexagonal boron nitride is only capable of reaching through its relative density of oversintering
70% or so, such as prepared application No. is a kind of 201410422994.6 pressureless sintering the method for high-purity hexagonal boron nitride ceramics with
High-purity hexagonal boron nitride powder is only 56% or so for the hexagonal boron nitride ceramic dense degree of raw material preparation, and in order to improve six side's nitrogen
Change the consistency of boron ceramics, most of method is to add sintering aid during the sintering process, such as B2O3、Y2O3、Al2O3、SiO2、
AlN etc. can reduce its high temperature although being increased by the hexagonal boron nitride consistency that addition sintering aid obtains
Service performance.Such as application No. is a kind of preparation method of 201410393724.7 high-compactness hexagonal boron nitride ceramic material its
It discloses in hBN powder surface coated Si O2Realize SiO2Sintering aid is uniformly distributed, and passes through discharge plasma sintering or heat
Isostatic sintering, obtains high-densit hBN block, but it is in hBN powder surface coated Si O2Process is complicated and its preparation
High-densit h-BN block consistency is only up to 86.4%, and compressive strength is up to 79MPa.
Summary of the invention
The technical problem to be solved by the invention is to provide a kind of high-intensitive boron nitride ceramics and preparation method thereof, this method
By being sintered the nano cubic boron nitride powder of single particle size, high-intensitive boron nitride ceramics is obtained.
In order to solve the above technical problems, the technical scheme adopted by the invention is that:
It is a kind of high intensity boron nitride ceramics preparation method, preparation method the following steps are included:
A it) charges: weighing the single particle size nano cubic boron nitride powder of certain mass, pre-molding, after pre-molding
Preformed compact be put into sintering mold；
B it) is sintered: the preformed compact in step A) is put into togerther discharging plasma sintering equipment or heat together with sintering mold
It is sintered in pressure agglomerating plant；
C it) discharges: taking out mold after temperature in equipment is cooled to room temperature, move back mould and obtain high-intensitive boron nitride ceramics block.
Technical solution of the present invention further improvement lies in that: in step A) sintering mold be graphite jig, preformed compact with
It is separated between graphite jig with graphite paper.
Technical solution of the present invention further improvement lies in that: in step A) pre-molding be two-way application pressure, pressure
Size is 5MPa~10MPa.
Technical solution of the present invention further improvement lies in that: the single particle size nano cubic boron nitride powder in step A)
Partial size be 10nm~500nm.
Technical solution of the present invention further improvement lies in that: sintering step is first to apply precompression in step B), is taken out true
Sky to vacuum degree is higher than 1 × 10-1Apply sintering pressure after Pa, pressure to be sintered is warming up to sintering temperature, high temperature sintering after stablizing
Heating schedule and release are closed afterwards.
Technical solution of the present invention further improvement lies in that: step B) in apply precompression be 5MPa~10MPa, burn
Knot pressure size is 30MPa~50MPa, and sintering temperature is 1400 DEG C~2000 DEG C, and soaking time is 1min~30min.
Technical solution of the present invention further improvement lies in that: in step B) sintering processing be discharge plasma sintering or
It is hot pressed sintering.
Technical solution of the present invention further improvement lies in that: step B) heat up rate be 50 DEG C/min~150 DEG C/
min。
Present invention also provides high-intensitive boron nitride ceramics, compressive strengths prepared by the preparation method to be not less than
500MPa, compression strain are not less than 8%.
By adopting the above-described technical solution, the technological progress achieved by the present invention is:
A kind of high-intensitive boron nitride ceramics of the present invention and preparation method thereof, this method is vertical by the nanometer of sintering single particle size
Square boron nitride powder obtains high-intensitive boron nitride ceramics.
Using the nano cubic boron nitride powder of single particle size, boron nitride powder is undergone phase transition during the sintering process, cube
Boron nitride powder volume surrounding occurs graphitization and becomes hexagonal boron nitride, and powder central part still retains cubic structure, and centre had
Degree mutually exists, and boron nitride ceramics made from the nano cubic boron nitride powder with single particle size, crystallite dimension is more consistent, micro-
Institutional framework distribution is more uniform, and consistency and intensity are also relatively high.
To the two-way application pressure of powder when pre-molding, nano cubic boron nitride powder in compression mould it is two-way by
Power reduces preformed compact two-way pressure gradient, avoids two-way pressure gradient caused by unidirectionally pressing excessive, and makes on preformed compact
Lower density difference is larger, and then influences the whole consistency of block after sintering, and two-way application pressure also can make powder compressed
It is finer and close, conducive to the sintering of subsequent preformed compact.
Sintering pressure is set as 30MPa~50MPa, which can control the phase velocity of cubic boron nitride, no
Powder is only set all not become hexagonal boron nitride after fully sintered, and it is too fast to prevent crystal grain from growing up, it is ensured that prepared
The consistency of boron nitride ceramics.
Graphite paper separates graphite jig and preformed compact, prevents preformed compact and graphite jig in sintering process sintered together
Cause to be difficult to move back mould and obtain block, also avoids forcing to remove block and damage graphite jig, the use of mold can be improved
Service life.
Detailed description of the invention
Fig. 1 (a) is the X-ray diffraction spectrum that the embodiment of the present invention 1 prepares product, and Fig. 1 (b) is prepared by the embodiment of the present invention 1
Product single compressing stress strain curve；
Fig. 2 (a) is the X-ray diffraction spectrum that the embodiment of the present invention 2 prepares product, and Fig. 2 (b) is prepared by the embodiment of the present invention 2
Product single compressing stress strain curve；
Fig. 3 (a) is the X-ray diffraction spectrum that the embodiment of the present invention 3 prepares product, and Fig. 3 (b) is prepared by the embodiment of the present invention 3
Product single compressing stress strain curve；
Fig. 4 (a) is the X-ray diffraction spectrum that the embodiment of the present invention 4 prepares product, and Fig. 4 (b) is prepared by the embodiment of the present invention 4
Product single compressing stress strain curve；
Fig. 5 (a) is the X-ray diffraction spectrum that the embodiment of the present invention 5 prepares product, and Fig. 5 (b) is prepared by the embodiment of the present invention 5
Product single compressing stress strain curve.
Specific embodiment
The present invention is described in further details below with reference to embodiment:
Embodiment 1
A kind of preparation method of high-intensitive boron nitride ceramics of the present embodiment the following steps are included:
A it) charges: weighing the single particle size nano cubic boron nitride powder of 2g, single particle size nano cubic boron nitride powder
Partial size be 50nm, pre-molding, pre-molding be two-way application pressure, pressure size 10MPa will be pre- after pre-molding
Green compact is put into sintering mold, and sintering mold is graphite jig, is separated between preformed compact and graphite jig with graphite paper；
B it) is sintered: the preformed compact in step A) is put into togerther discharging plasma sintering equipment sintering together with sintering mold,
Sintering processing is discharge plasma sintering, and sintering step is first to apply precompression, and precompression 10MPa is evacuated to vacuum degree
Higher than 1 × 10-1Apply sintering pressure after Pa, sintering pressure size is 30MPa, and pressure to be sintered is warming up to sintering temperature after stablizing
Degree, the rate of heating are 150 DEG C/min, and sintering temperature is 1600 DEG C, soaking time 4min, and heating journey is closed after high temperature sintering
Sequence and release；
Discharging plasma sintering equipment used in the present embodiment is the SPS-3.20MK- of Sumitomo Coal Mining K. K
IV；
C it) discharges: taking out mold after temperature in equipment is cooled to room temperature, move back mould and obtain high-intensitive boron nitride ceramics block.
The compressive strength that test of the present invention prepares product high intensity boron nitride ceramics uses material mechanical performance to test
Machine, test sample are cylindrical body, and test specimens column dimension is diameter 3mm, height 4.5mm.
High-intensitive boron nitride ceramics prepared by the preparation method of the high-intensitive boron nitride ceramics of the present embodiment is opaque
Block, the X-ray diffraction spectrum as shown in Fig. 1 (a), high-intensitive boron nitride ceramics block are by hexagonal boron nitride (hBN) and a small amount of
The nano-multicrystal bulk that cubic boron nitride (cBN) is constituted, as shown in Fig. 1 (b), the compressive strength of high-intensitive boron nitride ceramics block
For 935MPa, compression strain 12%.
Embodiment 2
A kind of preparation method of high-intensitive boron nitride ceramics of the present embodiment, processing step is close with embodiment 1, with reality
Example 1 is applied to differ shown in other specific process parameter arranges referring to embodiment 2 in table 1.
High-intensitive boron nitride ceramics prepared by the preparation method of the high-intensitive boron nitride ceramics of the present embodiment is opaque
Block, the X-ray diffraction spectrum as shown in Fig. 2 (a), high-intensitive boron nitride ceramics block are by hexagonal boron nitride (hBN) and a small amount of
The nano-multicrystal bulk that cubic boron nitride (cBN) is constituted, as shown in Fig. 2 (b), the compressive strength of high-intensitive boron nitride ceramics block
For 820MPa, compression strain 11%.
Embodiment 3
A kind of preparation method of high-intensitive boron nitride ceramics of the present embodiment, processing step is close with embodiment 1, with reality
Example 1 is applied to differ shown in other specific process parameter arranges referring to embodiment 3 in table 1.
High-intensitive boron nitride ceramics prepared by the preparation method of the high-intensitive boron nitride ceramics of the present embodiment is opaque
Block, the X-ray diffraction spectrum as shown in Fig. 3 (a), high-intensitive boron nitride ceramics block are by hexagonal boron nitride (hBN) and a small amount of
The nano-multicrystal bulk that cubic boron nitride (cBN) is constituted, as shown in Fig. 3 (b), the compressive strength of high-intensitive boron nitride ceramics block
For 707MPa, compression strain 10.3%.
Embodiment 4
A kind of preparation method of high-intensitive boron nitride ceramics of the present embodiment, processing step is close with embodiment 1, with reality
Example 1 is applied to differ shown in other specific process parameter arranges referring to embodiment 4 in table 1.
High-intensitive boron nitride ceramics prepared by the preparation method of the high-intensitive boron nitride ceramics of the present embodiment is opaque
Block, the X-ray diffraction spectrum as shown in Fig. 4 (a), high-intensitive boron nitride ceramics block are by hexagonal boron nitride (hBN) and a small amount of
The nano-multicrystal bulk that cubic boron nitride (cBN) is constituted, as shown in Fig. 4 (b), the compressive strength of high-intensitive boron nitride ceramics block
For 615MPa, compression strain 9.8%.
Embodiment 5
A kind of preparation method of high-intensitive boron nitride ceramics of the present embodiment, processing step is close with embodiment 1, with reality
Example 1 is applied to differ shown in other specific process parameter arranges referring to embodiment 5 in table 1.
High-intensitive boron nitride ceramics prepared by the preparation method of the high-intensitive boron nitride ceramics of the present embodiment is opaque
Block, the X-ray diffraction spectrum as shown in Fig. 5 (a), high-intensitive boron nitride ceramics block are by hexagonal boron nitride (hBN) and a small amount of
The nano-multicrystal bulk that cubic boron nitride (cBN) is constituted, as shown in Fig. 5 (b), the compressive strength of high-intensitive boron nitride ceramics block
For 520MPa, compression strain 8.8%.
The preparation method parameter lookup table of 1 Examples 1 to 5 high intensity boron nitride ceramics of table
2 Examples 1 to 5 high intensity boron nitride ceramics consistency of table and single compressing stress strain property parameter lookup table
Claims (9)
1. it is a kind of high intensity boron nitride ceramics preparation method, it is characterised in that: preparation method the following steps are included:
A it) charges: weighing the single particle size nano cubic boron nitride powder of certain mass, pre-molding will be pre- after pre-molding
Green compact is put into sintering mold；
B it) is sintered: the preformed compact in step A) being put into togerther discharging plasma sintering equipment together with sintering mold or hot pressing is burnt
It is sintered in knot equipment；
C it) discharges: taking out mold after temperature in equipment is cooled to room temperature, move back mould and obtain high-intensitive boron nitride ceramics block.
2. a kind of preparation method of high-intensitive boron nitride ceramics according to claim 1, it is characterised in that: step A) in burn
Knot mold is graphite jig, is separated between preformed compact and graphite jig with graphite paper.
3. a kind of preparation method of high-intensitive boron nitride ceramics according to claim 1, it is characterised in that: step A) in it is pre-
Molded is two-way application pressure, and pressure size is 5MPa ~ 10MPa.
4. a kind of preparation method of high-intensitive boron nitride ceramics according to claim 1, it is characterised in that: step A) in
The partial size of single particle size nano cubic boron nitride powder is 10nm ~ 500nm.
5. a kind of preparation method of high-intensitive boron nitride ceramics according to claim 1, it is characterised in that: step B) in burn
Knot step is first to apply precompression, is evacuated to vacuum degree higher than 1 × 10-1Apply sintering pressure after Pa, pressure to be sintered is stablized
After be warming up to sintering temperature, heating schedule and release are closed after high temperature sintering.
6. a kind of preparation method of high-intensitive boron nitride ceramics according to claim 5, it is characterised in that: step B) in apply
The precompression added is 5MPa ~ 10MPa, and sintering pressure size is 30MPa ~ 50MPa, and sintering temperature is 1400 DEG C ~ 2000 DEG C, heat preservation
Time is 1min ~ 30min.
7. a kind of preparation method of high-intensitive boron nitride ceramics according to claim 1, it is characterised in that: step B) in burn
Knot mode is discharge plasma sintering either hot pressed sintering.
8. a kind of preparation method of high-intensitive boron nitride ceramics according to claim 1, it is characterised in that: step B) heating
Rate be 50 DEG C/min ~ 150 DEG C/min.
9. high-intensitive boron nitride ceramics prepared by the described in any item preparation methods of claim 1 ~ 8, it is characterised in that: compression
Intensity is not less than 500MPa, and compression strain is not less than 8%.
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| CN111004036A (en) * | 2019-12-25 | 2020-04-14 | 中国科学院兰州化学物理研究所 | High-density hexagonal boron nitride-based solid lubricating composite material and preparation method thereof |
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| CN115594509A (en) * | 2022-09-27 | 2023-01-13 | 中国有色桂林矿产地质研究院有限公司（Cn） | Polycrystalline cubic boron nitride composite material with rod crystal structure and preparation method and application thereof |
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| CN111004036A (en) * | 2019-12-25 | 2020-04-14 | 中国科学院兰州化学物理研究所 | High-density hexagonal boron nitride-based solid lubricating composite material and preparation method thereof |
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| CN115594509A (en) * | 2022-09-27 | 2023-01-13 | 中国有色桂林矿产地质研究院有限公司（Cn） | Polycrystalline cubic boron nitride composite material with rod crystal structure and preparation method and application thereof |
| CN117142863A (en) * | 2023-10-31 | 2023-12-01 | 山东鹏程陶瓷新材料科技有限公司 | Boron nitride ceramic setter plate and preparation method thereof |
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