IE922291A1 - Process for preparing boron nitride ceramics - Google Patents
Process for preparing boron nitride ceramicsInfo
- Publication number
- IE922291A1 IE922291A1 IE229192A IE922291A IE922291A1 IE 922291 A1 IE922291 A1 IE 922291A1 IE 229192 A IE229192 A IE 229192A IE 922291 A IE922291 A IE 922291A IE 922291 A1 IE922291 A1 IE 922291A1
- Authority
- IE
- Ireland
- Prior art keywords
- boron nitride
- formula
- process according
- precursor
- tertiary amine
- Prior art date
Links
Classifications
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—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
- C04B35/58—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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/064—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with boron
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—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
- C04B35/58—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
- 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
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—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
- C04B35/58—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
- C04B35/584—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 silicon nitride
- C04B35/589—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 silicon nitride obtained from Si-containing polymer precursors or organosilicon monomers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G79/00—Macromolecular compounds obtained by reactions forming a linkage containing atoms other than silicon, sulfur, nitrogen, oxygen, and carbon with or without the latter elements in the main chain of the macromolecule
- C08G79/08—Macromolecular compounds obtained by reactions forming a linkage containing atoms other than silicon, sulfur, nitrogen, oxygen, and carbon with or without the latter elements in the main chain of the macromolecule a linkage containing boron
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Organic Chemistry (AREA)
- Structural Engineering (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Medicinal Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Polymers & Plastics (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Ceramic Products (AREA)
Abstract
Boron nitride ceramics and their precursors. These precursors are obtained by a reaction of hydrazine substituted by organosilyl groups with boron trichloride.
Description
The invention relates to a process for preparing boron nitride ceramics from precursors which are derived from hydrazine, and the ceramic precursors obtained in this process .
According to the invention, there is provided a process for preparing boron nitride ceramic, which process comprises:
1/ reacting a compound of formula (I)
R3Si ,N
(I) with m.BCl3 under conditions allowing the formation of a precursor comprising units of formula (II)
B - Ν.·- N τ ί I ! J(II
Cl Z SlR3 in which formulae the symbols R, which may be identical or different, each represent an organic radical which contains up to 12 carbon atoms and which may be selected in particular from alkyl, cycloalkyl and aryl radicals, the symbol Z may represent H or -SiR3, Y may represent Li or -SiRs and m may be equal to 1 or 2, and
2/ subjecting precursor comprising units of formula (II) to a pyrolysis until a product containing BN is obtained.
- 3 In formulae I and II, the radical R is advantageously an alkyl radical having 1 to 4 carbon atoms and, preferably, a methyl radical.
According to a variant of this process, the 5 compound of formula (I) and BC13 are reacted in particular in the presence of a tertiary amine with the aim of trapping HCl formed during the reaction, leading to the precursor (II) in the form of an amine hydrochloride.
The tertiary amine may be chosen from a wide range 10 of products corresponding to this definition. Triethylamine is advantageously used as the tertiary amine.
The amount of tertiary amine, when it is used, is suitably about one mole per mole of BC1,.
In the process according to the invention, implemented without tertiary amine, the mixture of compound of formula (I) + BC1, is generally carried out at low temperature (preferably lower than -50°C and more precisely between -70 and -100°C) in an organic solvent medium, which may for example be an alkane which is liquid at the reaction temperature, such as pentane. This temperature is generally maintained for between ten minutes and one hour.
After being returned to the vicinity of 0°C and after elimination of the solvent, optionally under reduced pressure, the precursor of formula II is obtained in the form of a white solid, soluble for example in pentane or toluene.
This solid may be pyrolysed directly, for example under an argon or ammonia atmosphere at a temperature
- 4 generally between 800 and 1500°C and preferably between 900 and 1200°C. This leads to a ceramic containing boron nitride .
Before pyrolysis, it is possible to subject the 5 precursor to a pretreatment, for example between 120 and
150°C, this pretreatment leading to a soluble vitreous white solid, or alternatively to subject the latter solid to a new treatment at a higher temperature, for example between 200 and 250°C, leading to a vitreous white solid soluble in pentane or toluene. A white insoluble solid may also be obtained by leaving the above solid at room temperature for several hours.
If the reaction is carried out in the presence of a tertiary amine, a precipitate of amine hydrochloride is formed, which may be eliminated for example by filtration.
The precursor is then generally present in the form of a gel, a treatment between 120 and 150°C leading to the vitreous soluble white solid mentioned above. This precursor may be pyrolysed in the temperature zone indicated above.
It may thus be noted that the process according to the invention leads to precursors which, by means of appropriate treatment, are crosslinked to a greater or lesser degree and may therefore be appropriate to the implementation conditions before moving to the final stage of totally insoluble product.
The following Example further illustrates the invention .
- 5 EXAMPLE
l.a./ 1.76 g of tris(trimethylsilyl)hydrazine is dissolved in 30 ml of pentane at room temperature and the solution is cooled to -80°C.
l.b./ A solution of 0.70 g of BC13 in 10 ml of pentane is added to this cooled solution. After ten minutes, the mixture is returned to room temperature. The solvent is eliminated and a white solid is obtained.
1. e./ The white solid is heated to 140°C for two hours under reduced pressure (1 mm Hg). After this treatment, a new vitreous white solid (II), soluble in pentane or toluene, is obtained.
2. a./ A solution of 2.15 g of tris(trimethylsilyl) hydrazine and 0.90 g of triethylamine in 30 ml of pentane may also be reacted with a solution of 1.01 g of BC13 in 10 ml of pentane to obtain a gel (same experimental conditions as those described above).
2. b./ The gel is heated to 140°C for two hours under reduced pressure (1 mm Hg). After this treatment, a soluble vitreous white solid (II) is obtained.
3. / The pyrolysis of II (at 1000°C for eight hours under a stream of ammonia or argon) leads to boron nitride in a yield of 25 %.
4. / If, at the end of the operation described under
l.b./, the soluble solid obtained is left for about ten hours at room temperature, conversion into a new insoluble white solid is observed. This white solid is heated to 140°C for
- 6 two hours under reduced pressure (1 mm Hg). The pyrolysis of the white solid obtained leads to a yield in boron nitride of to 37 %.
Claims (9)
1. Process for preparing boron nitride ceramic, which process comprises: 1/ reacting a compound of formula (I) (I) with m.BCl, under conditions allowing the formation of a precursor comprising units of formula (II) B - N - N L I I I Cl Z SiR 3 (II) in which formulae the symbols R, which may be identical or 10 different, each represent an organic radical which contains up to 12 carbon atoms, the symbol Z represents H or -SiR 3 , Y represents Li or -SiR 3 and m is equal to 1 or 2, and 2. / subjecting precursor comprising units of formula (II) to a pyrolysis until a product containing BN is 15 obtained.
2. Process according to claim 1, wherein each R repreesnts an alkyl, cycloalkyl or aryl radical.
3. Process according to Claim 1 or 2, wherein, in step 1, the reaction is carried out in the presence of a 20 tertiary amine.
4. . Process according to Claim 3, wherein the - 8 tertiary amine is used in an amount of about one mole of amine per mole of BC1 3 .
5. Process according to Claim 3 or 4, wherein the tertiary amine is triethylamine. 5
6. Process according to any one of the preceding claims wherein the precursor obtained in step 1 is subjected to pretreatment at between 120 and 150°C or at between 200 and 250°C and optionally left at room temperature prior to pyrolysis . 10
7. Process for preparing boron nitride ceramic substantially as described in the foregoing Example.
8. Boron nitride ceramic prepared by the process claimed in any one of the preceding claims.
9. Compound comprising units of formula (II) as 15 defined in claim 1.
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| FR9109046A FR2679228A1 (en) | 1991-07-17 | 1991-07-17 | PROCESS FOR THE PREPARATION OF CERAMICS OF BORON NITRIDE FROM PRECURSORS DERIVED FROM HYDRAZINE |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| IE922291A1 true IE922291A1 (en) | 1993-01-27 |
Family
ID=9415237
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| IE229192A IE922291A1 (en) | 1991-07-17 | 1992-07-14 | Process for preparing boron nitride ceramics |
Country Status (9)
| Country | Link |
|---|---|
| EP (1) | EP0524858A1 (en) |
| KR (1) | KR930002281A (en) |
| CN (1) | CN1071158A (en) |
| AU (1) | AU2036192A (en) |
| CA (1) | CA2074030A1 (en) |
| FR (1) | FR2679228A1 (en) |
| IE (1) | IE922291A1 (en) |
| IL (1) | IL102498A0 (en) |
| NO (1) | NO922778L (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2703040B1 (en) * | 1993-03-23 | 1995-05-12 | Atochem Elf Sa | Process for the preparation of powder for ceramic nitride and / or metallic carbide and / or metalloid by flash pyrolysis and the powder thus obtained. |
| JP2002231768A (en) * | 2001-02-01 | 2002-08-16 | Shinkawa Ltd | Inner lead bonding device |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2629463B1 (en) * | 1988-04-01 | 1990-12-14 | Rhone Poulenc Chimie | PROCESS FOR THE PREPARATION OF POLYMERS BASED ON BORON AND NITROGEN PRECURSORS OF BORON NITRIDE |
| FR2643358B1 (en) * | 1989-02-20 | 1991-11-22 | Rhone Poulenc Chimie | PROCESS FOR THE PREPARATION OF BORON NITRIDE |
-
1991
- 1991-07-17 FR FR9109046A patent/FR2679228A1/en active Pending
-
1992
- 1992-07-10 EP EP92402013A patent/EP0524858A1/en not_active Withdrawn
- 1992-07-14 IE IE229192A patent/IE922291A1/en not_active Application Discontinuation
- 1992-07-14 NO NO92922778A patent/NO922778L/en unknown
- 1992-07-15 IL IL102498A patent/IL102498A0/en unknown
- 1992-07-16 CA CA002074030A patent/CA2074030A1/en not_active Abandoned
- 1992-07-16 KR KR1019920012766A patent/KR930002281A/en not_active Application Discontinuation
- 1992-07-16 AU AU20361/92A patent/AU2036192A/en not_active Abandoned
- 1992-07-17 CN CN92108820A patent/CN1071158A/en active Pending
Also Published As
| Publication number | Publication date |
|---|---|
| CN1071158A (en) | 1993-04-21 |
| AU2036192A (en) | 1993-01-21 |
| NO922778L (en) | 1993-01-18 |
| FR2679228A1 (en) | 1993-01-22 |
| CA2074030A1 (en) | 1993-01-18 |
| KR930002281A (en) | 1993-02-22 |
| IL102498A0 (en) | 1993-01-14 |
| EP0524858A1 (en) | 1993-01-27 |
| NO922778D0 (en) | 1992-07-14 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| FC9A | Application refused sect. 31(1) |