CN107698264A - A kind of preparation method of modified alpha-phase silicon nitride powder - Google Patents
A kind of preparation method of modified alpha-phase silicon nitride powder Download PDFInfo
- Publication number
- CN107698264A CN107698264A CN201610644874.XA CN201610644874A CN107698264A CN 107698264 A CN107698264 A CN 107698264A CN 201610644874 A CN201610644874 A CN 201610644874A CN 107698264 A CN107698264 A CN 107698264A
- Authority
- CN
- China
- Prior art keywords
- silicon nitride
- nitride powder
- preparation
- purity
- silico briquette
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
- C04B35/622—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
- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/6261—Milling
-
- 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
Abstract
The invention belongs to inorganic non-metallic Preparation Technique of Powders field, and in particular to a kind of preparation method of modified alpha-phase silicon nitride powder.Its step is：High-purity silico briquette is finely ground to silica flour, is proportionally added into diluent mixing.By compound in vacuum high-temperature nitriding furnace, high pure nitrogen is passed through, nitridation reaction is carried out after being warming up to certain temperature.By react obtained nitridation silico briquette by crushing, fine grinding technology is levigate to ceramic grade powder requirement granularity, addition dispersant is modified to beta-silicon nitride powder during fine grinding.Beta-silicon nitride powder prepared by the present invention has good dispersiveness, and α phases are more than 90%, while ensure that the purity of generation beta-silicon nitride powder as initiation material using high-purity silico briquette, are advantageous to improve biscuit density and sintering activity in silicon nitride ceramics sintering process.
Description
Technical field
The invention belongs to inorganic non-metallic Preparation Technique of Powders field, and in particular to a kind of modified alpha-phase silicon nitride powder
Preparation method.
Background technology
Silicon nitride due to intensity height, good toughness, it is corrosion-resistant, wear-resistant, density is small the advantages that, and there is good heat resistanceheat resistant
Pinking and self lubricity, are received much concern in recent years, and critical role is occupied in new ceramics.Now have been supplied in refractory ceramics axle
Hold, anticorrosive wear-resistant part, high-speed cutting cutter, dehydration panel etc., be related to a variety of application fields such as machinery, electronics, military project.
The key for preparing the silicon nitride ceramics of function admirable is purity height, the silicon nitride powder that granularity is small, α phase contents are high
Body.Due to α-Si3N4Than β-Si3N4With higher sintering activity, typically require in powder α phases up to more than 90%.Common system
The method of standby beta-silicon nitride powder has self- propagating method, Si powder direct nitridation method, thermal decomposition method and carbothermic method.Wherein thermal decomposition method
Higher for equipment, technological requirement, large-scale production is relatively difficult, and only Ube uses the method at present.Carbothermic method
It is relatively easy with self- propagating method technique, but beta-silicon nitride powder impurity prepared by carbothermic method is higher, and self- propagating method process is not easy
Control, and nitrogen pressure（＞ 3MPa）Requirement for equipment is higher.And Si powder direct nitridation method can be in pressure-fired or normal pressure
Lower progress, it is relatively low to equipment requirement, it is the conventional method for preparing beta-silicon nitride powder of in the market.
Silicon nitride prepared by general silicon powder nitride is block, need to pass through crushing, ball-milling technology obtains ceramics small grain size
Beta-silicon nitride powder.Silicon nitride after ball milling typically has less granularity（0.4~1.4 μm）, and thinner beta-silicon nitride powder holds
Easily reunite.It is unfavorable for improving the consistency of base substrate in ceramic post sintering process, so as to influence ceramic dense degree and performance.
The content of the invention
It is an object of the invention to provide a kind of preparation method of modified alpha-phase silicon nitride powder, the beta-silicon nitride powder of preparation
With good dispersiveness, α phases are more than 90%, are advantageous to improve biscuit density in silicon nitride ceramics sintering process and sintering is lived
Property.The adopted technical solution is that：
（1）High-purity silico briquette is finely ground to silica flour, is proportionally added into diluent mixing；
（2）By compound in vacuum high-temperature nitriding furnace, high pure nitrogen is passed through, nitridation reaction is carried out after being warming up to certain temperature；
（3）By react obtained nitridation silico briquette by crushing, fine grinding technology is levigate to ceramic grade powder requirement granularity, fine grinding
Dispersant is added in journey to be modified to beta-silicon nitride powder.
Further, the silico briquette purity is 99.99%, and diluent is α-Si3N4Powder, silica flour are with diluent ratio
（10~40）:（90~60）, reaction temperature is 1350~1550 DEG C.
Further, the dispersant is ammonium polyacrylate, polyvinylpyrrolidone, ammonium polymethacrylate or citric acid
One kind in ammonium, using silicon nitride ball as ball-milling medium, with one kind in alcohol or deionized water for decentralized medium.
Further, any dispersant addition is 0.2~2%, and ratio of grinding media to material is（3~10）：1.
Beneficial effects of the present invention：The present invention is controlled certain with being mixed into raw material with diluent after high-purity silico briquette ball milling
Nitridation silicon bulk is prepared in reaction temperature, then is finely ground to beta-silicon nitride powder through crushing, ball-milling technology.Added in mechanical milling process
A certain amount of dispersant is modified to beta-silicon nitride powder.There is obtained beta-silicon nitride powder good dispersiveness, α phases to be more than
90%, while the purity for generating beta-silicon nitride powder is ensure that as initiation material using high-purity silico briquette, it is sintered in silicon nitride ceramics
Be advantageous to improve biscuit density and sintering activity in journey.
Brief description of the drawings
Fig. 1 is the XRD for the beta-silicon nitride powder being prepared using the technique of the present invention.
Fig. 2 is the SEM figures for the beta-silicon nitride powder being prepared using the technique of the present invention.
Embodiment
Embodiment 1
High-purity silicon powder after ball milling and diluent are pressed 20:80 ratio mixing, nitridation reaction preparation is carried out in 1450 DEG C of temperature
Obtain nitrogenizing silicon bulk.To nitrogenize silicon bulk be crushed to ammonium polyacrylate is added after certain particle size, alcohol is levigate to 0.9 μm of nitrogen
SiClx powder.It is 92% that powder, which has good dispersiveness, α phase silicon nitrides content,.
Embodiment 2
High-purity silicon powder after ball milling and diluent are pressed 35:65 ratio mixing, nitridation reaction preparation is carried out in 1500 DEG C of temperature
Obtain nitrogenizing silicon bulk.Nitridation silicon bulk is crushed to after certain particle size and adds polyvinylpyrrolidone, deionized water is levigate extremely
0.7 μm of beta-silicon nitride powder.It is 93.6% that powder, which has good dispersiveness, α phase silicon nitrides content,.
Claims (5)
1. a kind of preparation method of modified alpha-phase silicon nitride powder, its feature comprise the following steps：
（1）High-purity silico briquette is finely ground to silica flour, is proportionally added into diluent mixing；
（2）By compound in vacuum high-temperature nitriding furnace, high pure nitrogen is passed through, nitridation reaction is carried out after being warming up to certain temperature；
（3）By react obtained nitridation silico briquette by crushing, fine grinding technology is levigate to ceramic grade powder requirement granularity, fine grinding
Dispersant is added in journey to be modified beta-silicon nitride powder.
2. the preparation method of a kind of modified alpha-phase silicon nitride powder according to claim 1, it is characterised in that in step 1
The silico briquette purity is 99.99%, and diluent is α-Si3N4Powder, silica flour are with diluent ratio（10~40）:（90~60）.
3. the preparation method of a kind of modified alpha-phase silicon nitride powder according to claim 1, it is characterised in that in step 2
The nitridation reaction temperature is 1350~1550 DEG C.
4. the preparation method of a kind of modified alpha-phase silicon nitride powder according to claim 1, it is characterised in that in step 3
The dispersant is one kind in ammonium polyacrylate, polyvinylpyrrolidone, ammonium polymethacrylate or ammonium citrate, with nitridation
Silicon ball is ball-milling medium, with one kind in alcohol or deionized water for decentralized medium.
5. the preparation method of a kind of modified alpha-phase silicon nitride powder according to claim 4, it is characterised in that described
A kind of dispersant addition is 0.2~2%, and ratio of grinding media to material is（3~10）：1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610644874.XA CN107698264A (en) | 2016-08-09 | 2016-08-09 | A kind of preparation method of modified alpha-phase silicon nitride powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610644874.XA CN107698264A (en) | 2016-08-09 | 2016-08-09 | A kind of preparation method of modified alpha-phase silicon nitride powder |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107698264A true CN107698264A (en) | 2018-02-16 |
Family
ID=61168748
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610644874.XA Pending CN107698264A (en) | 2016-08-09 | 2016-08-09 | A kind of preparation method of modified alpha-phase silicon nitride powder |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107698264A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108557780A (en) * | 2018-04-27 | 2018-09-21 | 浙江东瓷新材料有限公司 | A kind of preparation method of beta-silicon nitride powder |
| CN113493191A (en) * | 2020-04-08 | 2021-10-12 | 新疆晶硕新材料有限公司 | Method for preparing high-purity alpha-silicon nitride powder and high-purity alpha-silicon nitride powder |
| CN116216662A (en) * | 2023-02-01 | 2023-06-06 | 江苏富乐华功率半导体研究院有限公司 | Synthesis method of silicon nitride powder |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1362358A (en) * | 2002-01-22 | 2002-08-07 | 清华大学 | Low pressure combustion process of synthesizing alpha-phase silicon nitride powder |
| CN102173396A (en) * | 2011-01-25 | 2011-09-07 | 巩义市宏泰氮化硅材料有限公司 | Production method of high-content alpha-crystal form silicon nitride powders |
| CN102173397A (en) * | 2011-01-25 | 2011-09-07 | 巩义市宏泰氮化硅材料有限公司 | Production method of high-content silicon nitride (Si3N4) powder |
| CN107399973A (en) * | 2016-05-20 | 2017-11-28 | 河北高富氮化硅材料有限公司 | The technique that a kind of direct nitridation method prepares aluminium nitride powder |
-
2016
- 2016-08-09 CN CN201610644874.XA patent/CN107698264A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1362358A (en) * | 2002-01-22 | 2002-08-07 | 清华大学 | Low pressure combustion process of synthesizing alpha-phase silicon nitride powder |
| CN102173396A (en) * | 2011-01-25 | 2011-09-07 | 巩义市宏泰氮化硅材料有限公司 | Production method of high-content alpha-crystal form silicon nitride powders |
| CN102173397A (en) * | 2011-01-25 | 2011-09-07 | 巩义市宏泰氮化硅材料有限公司 | Production method of high-content silicon nitride (Si3N4) powder |
| CN107399973A (en) * | 2016-05-20 | 2017-11-28 | 河北高富氮化硅材料有限公司 | The technique that a kind of direct nitridation method prepares aluminium nitride powder |
Non-Patent Citations (3)
| Title |
|---|
| 姚守信编著: "《无机精细化工》", 31 March 1994, 成都：四川大学出版社 * |
| 殷声主编: "《燃烧合成》", 1999063, 北京：冶金工业出版社 * |
| 汪啸穆主编: "《陶瓷工艺学》", 31 May 1994, 北京：中国轻工业出版社 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108557780A (en) * | 2018-04-27 | 2018-09-21 | 浙江东瓷新材料有限公司 | A kind of preparation method of beta-silicon nitride powder |
| CN108557780B (en) * | 2018-04-27 | 2019-07-23 | 浙江东瓷新材料有限公司 | A kind of preparation method of beta-silicon nitride powder |
| CN113493191A (en) * | 2020-04-08 | 2021-10-12 | 新疆晶硕新材料有限公司 | Method for preparing high-purity alpha-silicon nitride powder and high-purity alpha-silicon nitride powder |
| CN113493191B (en) * | 2020-04-08 | 2022-11-22 | 新疆晶硕新材料有限公司 | Method for preparing high-purity alpha-silicon nitride powder and high-purity alpha-silicon nitride powder |
| CN116216662A (en) * | 2023-02-01 | 2023-06-06 | 江苏富乐华功率半导体研究院有限公司 | Synthesis method of silicon nitride powder |
| CN116216662B (en) * | 2023-02-01 | 2023-10-27 | 江苏富乐华功率半导体研究院有限公司 | Synthesis method of silicon nitride powder |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103130506B (en) | Method for preparing superfine titanium carbonitride | |
| CN102060535B (en) | Method for preparing high-purity Ti3AlC2 ceramics | |
| CN108529576B (en) | Silicon nitride and preparation method thereof | |
| Yang et al. | Synthesis of ultrafine ZrB 2 powders by sol-gel process | |
| CN107698264A (en) | A kind of preparation method of modified alpha-phase silicon nitride powder | |
| CN106631033A (en) | Method for preparing ZrB2 powder | |
| CN101863663B (en) | Combustion method for preparing submicron grade titanium carbide polycrystal powder | |
| CN115093233A (en) | Preparation method of high-purity superfine transition metal carbonitride high-entropy ceramic powder suitable for industrial mass production | |
| CN110256078A (en) | A kind of dopen Nano polycrystalline diamond and preparation method thereof | |
| CN107473237A (en) | A kind of preparation method of binary tungsten boride superhard material | |
| CN103848625B (en) | A kind ofly prepare the method with Rod-like shape zirconium boride powder | |
| CN111115592B (en) | Preparation method of nano silicon nitride powder | |
| CN106565246B (en) | A method of preparing aluminium nitride/yttrium nitride composite powder | |
| CN109437917B (en) | Method for producing titanium nitride and titanium carbonitride by two-stage reduction nitridation | |
| CN108455623A (en) | A kind of ultra fine transition metal boride powder and its preparation method and application | |
| CN107285288A (en) | The preparation method of nano silicon nitride powders | |
| CN102583380B (en) | High-temperature and high-pressure preparation method of carbide of molybdenum | |
| US7267808B2 (en) | Aluminum nitride powder, method for producing the same and use thereof | |
| CN107285329B (en) | Tungsten diboride hard material and preparation method and application thereof | |
| JP2005194154A (en) | Sialon sintered compact | |
| CN107043260A (en) | A kind of novel tertiary osmium rhenium diboride (Os1 xRexB2) hard material and preparation method thereof | |
| CN110483057A (en) | A kind of four tungsten boride materials and the preparation method and application thereof adulterating tantalum element | |
| CN107399973A (en) | The technique that a kind of direct nitridation method prepares aluminium nitride powder | |
| US10112833B2 (en) | Method for preparing aluminum nitride | |
| CN105439162B (en) | A kind of coarse grain diameter MO2Powder synthesizes thin MB2Raw powder's production technology |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20180216 |
|
| WD01 | Invention patent application deemed withdrawn after publication |