CN106747467A - A kind of preparation method of BN (C) ceramics - Google Patents
A kind of preparation method of BN (C) ceramics Download PDFInfo
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- CN106747467A CN106747467A CN201611030442.6A CN201611030442A CN106747467A CN 106747467 A CN106747467 A CN 106747467A CN 201611030442 A CN201611030442 A CN 201611030442A CN 106747467 A CN106747467 A CN 106747467A
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- C04B35/583—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on boron nitride
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- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
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Abstract
The invention provides a kind of preparation method of BN (C) ceramics, belong to ceramic preparation technical field.Step one, hexagonal boron nitride powder, graphite powder and lanthanum hexaboride powder are weighed respectively for raw material；Step 2, the raw material that will be weighed are fitted into ball grinder, and carrying out high-energy ball milling under argon gas atmosphere protection obtains BN (C) ceramic composite powder；Wherein ball material mass ratio is (5~50):1, ball radius are 4~8mm, and Ball-milling Time is 5~40h；Step 3, the ceramic composite powder that will be obtained in step 2 carry out high-pressure sinter and obtain BN (C) ceramic material.The preparation of BN (C) ceramic material of the invention is based on mechanical alloying and high pressure sintering process, and the preparation method is simple, and short preparation period, raw material is easy to get, cheap, environmental protection；The densification of BN (C) ceramic material of the invention is completed by high-pressure sinter, and sintering temperature is low, considerably reduces energy consumption；Crystal grain tends to equiaxial growth in BN (C) ceramic material of the invention, without substantially laminar structured.
Description
Technical field
The present invention relates to a kind of preparation method of BN (C) ceramics, belong to the preparation method technical field of BN (C) ceramics.
Background technology
Six side's boron nitrogen carbon ceramic materials have it is laminar structured, with corrosion-resistant, anti-oxidant, density is low, high temperature resistant and
The advantages of wave is good, has in fields such as high-temperature structural components, composite enhancing phase, kollag, catalyst carriers
The prospect of being widely applied.Most of research reports are all concentrated on and prepare powder or fibre using organic precursor method cracking process at present
Dimension.But can be used to prepare the precursor of BN (C) material, especially the high-purity and precursor with good mouldability has very much
Limit, it is expensive and poisonous, it is unfavorable for application and development of BN (C) ceramic material in industrial circle.
The content of the invention
The invention aims to solve the problems, such as above-mentioned prior art, i.e., most of research reports all collect at present
In in preparing powder or fiber using organic precursor method cracking process.But can be used to prepare the precursor of BN (C) material, especially
It is the high-purity and precursor with good mouldability is very limited, it is expensive and poisonous, it is unfavorable for that BN (C) ceramic material exists
The problem of application and development in industrial circle, and then a kind of preparation method of BN (C) ceramics is provided.
The purpose of the present invention is achieved through the following technical solutions：
A kind of preparation method of BN (C) ceramics, step is as follows：
Step one, hexagonal boron nitride powder, graphite powder and lanthanum hexaboride powder are weighed respectively for raw material；
Step 2, the raw material that will be weighed are fitted into ball grinder, and carrying out high-energy ball milling under argon gas atmosphere protection obtains BN (C)
Ceramic composite powder；Wherein ball material mass ratio is (5~50):1, ball radius are 4~8mm, and Ball-milling Time is 5~40h；
Step 3, the ceramic composite powder that will be obtained in step 2 carry out high-pressure sinter and obtain BN (C) ceramic material.
Beneficial effects of the present invention：First, the preparation of BN (C) ceramic material of the invention is based on mechanical alloying and high pressure combustion
Knot technique, the preparation method is simple, and short preparation period, raw material is easy to get, cheap, environmental protection；2nd, BN (C) of the invention
The densification of ceramic material is completed by high-pressure sinter, and sintering temperature is low, considerably reduces energy consumption；3rd, BN (C) of the invention
Crystal grain tends to equiaxial growth in ceramic material, without substantially laminar structured.
Brief description of the drawings
Fig. 1 is the XRD spectrum of the boron nitrogen carbon ceramic material that preparation method of the present invention is obtained.
Fig. 2 is the Fracture scan photo of the boron nitrogen carbon ceramic material that preparation method of the present invention is obtained.
Specific embodiment
The present invention is described in further detail below：The present embodiment enters under premised on technical solution of the present invention
Row is implemented, and gives detailed implementation method, but protection scope of the present invention is not limited to following embodiments.
Embodiment 1
A kind of preparation method of BN (C) ceramics involved by the present embodiment, step is as follows：
Step one, hexagonal boron nitride powder, graphite powder and lanthanum hexaboride powder are weighed respectively for raw material；
Step 2, the raw material that will be weighed are fitted into ball grinder, and carrying out high-energy ball milling under argon gas atmosphere protection obtains BN (C)
Ceramic composite powder；Wherein ball material mass ratio is (5~50):1, ball radius are 4~8mm, and Ball-milling Time is 5~40h；
Step 3, the ceramic composite powder that will be obtained in step 2 carry out high-pressure sinter and obtain BN (C) ceramic material.
In the step one, the purity of boron nitride powder is 99%~99.9%, and the particle diameter of boron nitride powder is 1~20 μm；Stone
The purity of ink powder is 99%~99.9%, and the particle diameter of graphite powder is 1~20 μm；The purity of lanthanum hexaboride powder be 99%~
99.9%, the particle diameter of lanthanum hexaboride powder is 10~50 μm.
In the step one, B:C:The mol ratio of N is 1:1:1, LaB6Addition for raw material gross mass 0.5~
5wt%.
In the step 2, ball material mass ratio is (10~40):1, ball radius be 6~7mm, Ball-milling Time be 10~
30h。
In the step 3, high-pressure sinter temperature be 1000~1600 DEG C, pressure be 1~8GPa, soaking time be 5~
25min。
Embodiment 2
A kind of preparation method of BN (C) ceramics involved by the present embodiment, step is as follows：First, according to B:C:N mol ratios are
1:1:1 ratio weighs hexagonal boron nitride powder and graphite powder；The LaB of 2wt% is weighed again6Powder；Wherein graphite purity is 99%
~99.9%, particle diameter is 15 μm；Boron nitride purity is 99%~99.9%, and particle diameter is 15 μm；Lanthanum hexaboride purity be 99%~
99.9%, particle diameter is 30 μm；2nd, the raw material that will be weighed is fitted into ball grinder, and high-energy ball milling is carried out i.e. under argon gas atmosphere protection
Can obtain and contain LaB6BN (C) ceramic composite powder；Wherein ball material mass ratio is 15:1, ball radius are 8mm, Ball-milling Time
It is 25h；3rd, laminar structured BN (C) is obtained by the composite granule that will be obtained in step 2 carries out discharge plasma sintering
Ceramic material；Wherein sintering temperature is 1400 DEG C, and pressure is 5GPa, and soaking time is 10min.
Fig. 1 is that (■ represents BN (C) crystalline phase, ▲ table for the XRD spectrum of the boron nitrogen carbon ceramic material that preparation method of the present invention is obtained
Show La5B2C6Crystalline phase, ★ represents the boron/carbon/nitrogen compound of La), the BN for being obtained after high temperature sintering of the present invention as shown in Figure 1
(C) ceramic material is mainly mutually made up of BN (C), additionally contains the compound of a small amount of La.
Laminar structured BN (C) ceramic materials obtained to preparation method of the present invention understand through analysis test, of the invention
The consistency of BN (C) ceramic material that preparation method is obtained is 76.0%, without substantially laminar structured.
Fig. 2 is the Fracture scan photo of the boron nitrogen carbon ceramic material that preparation method of the present invention is obtained, and be can be observed by Fig. 2
A small amount of sheet BN (C) crystal grain, most of BN (C) crystal grain do not have obvious laminar structured (only a small amount of), but become
In equiaxial growth.This is due to each oriented growth of BN (C) crystal grain to impartial pressure restraining in high pressure sintering processes.
Laminar structured BN (C) ceramic materials obtained to preparation method of the present invention understand through analysis test, of the invention
The consistency of BN (C) ceramic material that preparation method is obtained is 81.2%, without substantially laminar structured.
The above, preferably specific embodiment only of the invention, these specific embodiments are all based on the present invention
Different implementations under general idea, and protection scope of the present invention is not limited thereto, it is any to be familiar with the art
Technical staff the invention discloses technical scope in, the change or replacement that can be readily occurred in should all be covered of the invention
Within protection domain.Therefore, protection scope of the present invention should be defined by the protection domain of claims.
Claims (5)
1. the preparation method of a kind of BN (C) ceramics, it is characterised in that
Step one, hexagonal boron nitride powder, graphite powder and lanthanum hexaboride powder are weighed respectively for raw material；
Step 2, the raw material that will be weighed are fitted into ball grinder, high-energy ball milling is carried out under argon gas atmosphere protection and obtains BN (C) ceramics
Composite powder；Wherein ball material mass ratio is 5~50:1, ball radius are 4~8mm, and Ball-milling Time is 5~40h；
Step 3, the ceramic composite powder that will be obtained in step 2 carry out high-pressure sinter and obtain BN (C) ceramic material.
2. the preparation method of BN (C) according to claim 1 ceramics, it is characterised in that in the step one, boron nitride powder
Purity be 99%~99.9%, the particle diameter of boron nitride powder is 1~20 μm；The purity of graphite powder is 99%~99.9%, graphite
The particle diameter of powder is 1~20 μm；The purity of lanthanum hexaboride powder is 99%~99.9%, and the particle diameter of lanthanum hexaboride powder is 10~50 μm.
3. the preparation method of BN (C) according to claim 1 ceramics, it is characterised in that in the step one, B:C:N's
Mol ratio is 1:1:1, LaB6Addition for raw material gross mass 0.5~5wt%.
4. the preparation method of BN (C) according to claim 1 ceramics, it is characterised in that in the step 2, ball material quality
Than being 10~40:1, ball radius are 6~7mm, and Ball-milling Time is 10~30h.
5. the preparation method of BN (C) according to claim 1 ceramics, it is characterised in that in the step 3, high-pressure sinter
Temperature is 1000~1600 DEG C, and pressure is 1~8GPa, and soaking time is 5~25min.
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| CN201611030442.6A CN106747467A (en) | 2016-11-16 | 2016-11-16 | A kind of preparation method of BN (C) ceramics |
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| CN201611030442.6A CN106747467A (en) | 2016-11-16 | 2016-11-16 | A kind of preparation method of BN (C) ceramics |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112521160A (en) * | 2020-12-29 | 2021-03-19 | 山东硅纳新材料科技有限公司 | B4C/h-BN high-temperature complex-phase ceramic and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1907906A (en) * | 2005-08-05 | 2007-02-07 | 李根法 | Eutectic powder additive for producing ceram and ceramic solder and preparation method thereof |
| CN102674874A (en) * | 2012-05-31 | 2012-09-19 | 哈尔滨工业大学 | ZrC-SiC-LaB6 ternary superhigh temperature ceramic composite material and preparation method thereof |
-
2016
- 2016-11-16 CN CN201611030442.6A patent/CN106747467A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1907906A (en) * | 2005-08-05 | 2007-02-07 | 李根法 | Eutectic powder additive for producing ceram and ceramic solder and preparation method thereof |
| CN102674874A (en) * | 2012-05-31 | 2012-09-19 | 哈尔滨工业大学 | ZrC-SiC-LaB6 ternary superhigh temperature ceramic composite material and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| BIN LIANG: "Si-B-C-N monoliths with LaB6-induced well-developed BN(C) flakes", 《MATERIALS LETTERS》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112521160A (en) * | 2020-12-29 | 2021-03-19 | 山东硅纳新材料科技有限公司 | B4C/h-BN high-temperature complex-phase ceramic and preparation method thereof |
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