CN1146375A - 氮化硅的自研磨 - Google Patents

氮化硅的自研磨 Download PDF

Info

Publication number
CN1146375A
CN1146375A CN96109404A CN96109404A CN1146375A CN 1146375 A CN1146375 A CN 1146375A CN 96109404 A CN96109404 A CN 96109404A CN 96109404 A CN96109404 A CN 96109404A CN 1146375 A CN1146375 A CN 1146375A
Authority
CN
China
Prior art keywords
silicon nitride
liquid
weight
grind
suspended substance
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
Application number
CN96109404A
Other languages
English (en)
Inventor
D·斯蒂尔
W·沃尔科
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Hoechst AG
Original Assignee
Hoechst AG
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Hoechst AG filed Critical Hoechst AG
Publication of CN1146375A publication Critical patent/CN1146375A/zh
Pending legal-status Critical Current

Links

Images

Classifications

    • 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
    • C01B21/068—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 silicon
    • C01B21/0687—After-treatment, e.g. grinding, purification
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C23/00—Auxiliary methods or auxiliary devices or accessories specially adapted for crushing or disintegrating not provided for in preceding groups or not specially adapted to apparatus covered by a single preceding group
    • B02C23/06—Selection or use of additives to aid disintegrating
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C17/00—Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls
    • B02C17/16—Mills in which a fixed container houses stirring means tumbling the charge
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C23/00—Auxiliary methods or auxiliary devices or accessories specially adapted for crushing or disintegrating not provided for in preceding groups or not specially adapted to apparatus covered by a single preceding group
    • B02C23/18—Adding fluid, other than for crushing or disintegrating by fluid energy
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
    • F16K—VALVES; TAPS; COCKS; ACTUATING-FLOATS; DEVICES FOR VENTING OR AERATING
    • F16K25/00—Details relating to contact between valve members and seats
    • F16K25/005—Particular materials for seats or closure elements
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/80—Compositional purity

Landscapes

  • Engineering & Computer Science (AREA)
  • Food Science & Technology (AREA)
  • General Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Disintegrating Or Milling (AREA)
  • Grinding-Machine Dressing And Accessory Apparatuses (AREA)
  • Crushing And Grinding (AREA)
  • Ceramic Products (AREA)
  • Mechanical Treatment Of Semiconductor (AREA)

Abstract

本发明涉及一种氮化硅的研磨方法，所述氮化硅以悬浮体形式存在于液体中，其中研磨是自生进行的，并且氮化硅在悬浮体中的比例至少为30％(重量)。本发明优点在于工艺简单、廉价，并且可提高研磨后氮化硅的质量。

Description

氮化硅的自研磨
本发明涉及一种氮化硅的自研磨方法，其中氮化硅以悬浮体形式存在于液体中。
这类方法是已经为人们所知的，例如由DE4200085A1(D1)和DE4220014A1(D2)中可以了解到。
D1描述了一种制备具有烧结活性的Si3N4的方法，其中Si3N4原料通过湿磨在含水悬浮体中被粉碎。该方法是在装有研磨介质的容器中进行的，例如使用钢或Si3N4球作研磨介质在搅拌式球磨机或环形-间隙式(annular-gap)球磨机中进行。
在D2所述的方法中，待研磨的材料以悬浮体形式存在于液体中，该液体挥发后不留下任何残留物，可以是例如制冷剂，但这种方法通常也在装有研磨介质的设备中进行的。
已和原方法有以下缺点，就是由研磨介质中磨下的物料会污染研磨的产品，例如，当研磨介质是钢时，和/或不利地改变研磨产品的粒径分布。此外，研磨介质的磨损也增加了运行成本。
因此，本发明的目的之一就是提供一种如前面所述类型的自研磨方法，它无需使用研磨介质。
现已发现如果氧化硅在浮悬体中的比例至少为30％(重量)，则它就可以自研磨，即无需使用另外的研磨介质。本发明的目的通过前面所述的方法得以实现，其中研磨是自生进行的，并且氮化硅在悬浮体中的比例至少为30％(重量)。
因而，本发明提供了一种氮化硅的研磨方法，其中氮化硅以悬浮体形式存在于液体中，所述研磨是自生进行的，并且氮化硅在悬浮体中的比例至少为30％(重量)。氮化硅含量至少50％(重量)是有利的，60％(重量)则更好，70％(重量)是特别优选的。
在本发明的一个优选方案中，所述液体在挥发后不留下残留物。
在本发明的又一个优选方案中，研磨是在搅拌磨中进行的。
在本发明的另一个优选方案中，所用的氮化硅在悬浮体中的比例至少为50％(重量)，更优选60％(重量)，特别优选70％(重量)。
在本发明的再一个优选方案中，所用的氮化硅原料是直径d50小于10μm的颗粒状材料。
权利要求书中所述的单个技术特征或单个技术特征的组合也可形成本发明的独立方案，并且权利要求书中的技术特征也可以自由组合。
本发明方法的优点是明显的，它使研磨更加简单和廉价，并能提高产品质量。
在一个特殊方案中，悬浮液含有挥发后不留下残留物的液体，优选地是一种制冷剂液体，特别优选氮或氧或氩或氢或氦，或者为一种固体和液体二氧化碳的混合物或者为一种固体二氧化碳和液氮的混合物。
附图借助流程框图说明了本发明的一个示范性实例。
附图示出了一种用于氮化硅自研磨的工厂，它是根据本发明的一个特定方案而设计的，其中液氮用作形成悬浮体的液体。该工厂包括一个磨1，混合容器2，螺旋进料机3，过滤器4。磨1，混合容器2和螺旋进料机3分别由马达5，6和7驱动。物料的流动方向在图中以箭头表示，而不再另行标明。
待研磨的氮化硅作为原料从螺旋进料机3连续喂入，到达混合容器2。同时，液氮通过管线8和阀门9(带流量调节)(LIC)也进入混合容器2。在该容器中，由待研磨的氮化硅和液氮混合形成悬浮体。为了防止由于密度不同而引起的分层，优选通过马达6对混合容器2中的悬浮体进行剧烈搅拌。用泵11将悬浮体通过管线10送至磨1中。泵11最好带流量调节器(LIC)。在磨1中，氢化硅被很细地研磨，然后，通过管线12送到过滤器4中。在那里形成的气态氮通过管线13排出，而磨细的不含氮的产品通过管线14而取出，余下的液氮通过管线15和泵16返回至混合容器2中。
根据本发明，使用液氮进行氮化硅自研磨的工艺参数如下。
磨容积(升)              4
氮化硅原料的d50(μm)   2.37
转速(分钟-1)               2400
固含量(％重量)              60
产量(公斤/小时)             50
终产物的d50(μm)           0.86
使用水作悬浮介质的类似研磨试验按以下参数进行：氮化硅原料的d50(μm)       3         3        3转速(分钟-1)               2400      2400     2400固含量(％重量)              50        60       70产量(公斤/小时)             50        50       50终产物的d50(μm)           1.17      0.86     0.56
用本发明方法制得的氮化硅可用于许多工业领域，例如用来制造阀门。

Claims (7)

1.一种氮化硅的研磨方法，所述氮化硅以悬浮体形式存在于液体中，其中研磨是自生进行的，并且氮化硅在悬浮体中存在的比例至少为30％(重量)。
2.根据权利要求1的方法，其中所述的液体在挥发后不留下残留物。
3.根据权利要求1的方法，其中挥发后不留残留物的液体是一种制冷剂液体，优选地为氮或氧或氩或氢或氦，或者是一种固体和液体二氧化碳的混合物，或者是一种固体二氧化碳和液氮的混合物。
4.根据权利要求1的方法，其中研磨是在搅拌磨中进行的。
5.根据权利要求1的方法，其中所用的氮化硅是直径d50小于10μm的颗粒材料。
6.根据权利要求1的方法，其中所用的氮化硅在悬浮体中的比例至少为50％(重量)，优选60％(重量)，特别优选70％(重量)。
7.由权利要求1的方法获得的氮化硅用于制造阀门。
CN96109404A 1995-08-08 1996-08-08 氮化硅的自研磨 Pending CN1146375A (zh)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE19528958A DE19528958A1 (de) 1995-08-08 1995-08-08 Autogenes Mahlen von Siliziumnitrid
DE19528958.7 1995-08-08

Publications (1)

Publication Number Publication Date
CN1146375A true CN1146375A (zh) 1997-04-02

Family

ID=7768877

Family Applications (1)

Application Number Title Priority Date Filing Date
CN96109404A Pending CN1146375A (zh) 1995-08-08 1996-08-08 氮化硅的自研磨

Country Status (9)

Country Link
EP (1) EP0757922A3 (zh)
JP (1) JPH09142814A (zh)
KR (1) KR970009890A (zh)
CN (1) CN1146375A (zh)
BR (1) BR9603341A (zh)
CA (1) CA2182839A1 (zh)
DE (1) DE19528958A1 (zh)
TW (1) TW343162B (zh)
ZA (1) ZA966704B (zh)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113399093A (zh) * 2021-07-30 2021-09-17 深圳陶陶科技有限公司 机械破碎法制备类球形粉体的方法和类球形粉体

Family Cites Families (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR1094977A (fr) * 1953-11-28 1955-05-25 Installation de broyage à très basse température en présence de gaz liquéfiés
GB1310222A (en) * 1969-05-15 1973-03-14 English Clays Lovering Pochin Treatment of minerals
US4932166A (en) * 1986-05-30 1990-06-12 The Carborundum Company Inert autogenous attrition grinding
DE4113885A1 (de) * 1991-04-27 1992-10-29 Hoechst Ag Verfahren zur herstellung von feinteiligem kristallinem siliciumnitrid
DE4200085C2 (de) 1992-01-03 1997-04-17 Bayer Ag Verfahren zur Herstellung von sinteraktiven Si¶3¶-N¶4¶-Pulvern
DE4220014A1 (de) 1992-06-19 1993-12-23 Messer Griesheim Gmbh Verfahren zur Feinmahlung in Apparaten mit Mahlkörpern
DE4432153A1 (de) * 1994-09-09 1996-03-14 Evv Vermoegensverwaltungs Gmbh Verfahren und Vorrichtung zum kontinuierlichen autogenen Mahlen eines fließfähigen Behandlungsguts

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113399093A (zh) * 2021-07-30 2021-09-17 深圳陶陶科技有限公司 机械破碎法制备类球形粉体的方法和类球形粉体
CN113399093B (zh) * 2021-07-30 2023-08-11 深圳陶陶科技有限公司 机械破碎法制备类球形粉体的方法和类球形粉体

Also Published As

Publication number Publication date
TW343162B (en) 1998-10-21
EP0757922A3 (de) 1997-03-19
MX9603256A (es) 1997-07-31
EP0757922A2 (de) 1997-02-12
JPH09142814A (ja) 1997-06-03
DE19528958A1 (de) 1997-02-13
ZA966704B (en) 1997-02-10
KR970009890A (ko) 1997-03-27
BR9603341A (pt) 1998-05-05
CA2182839A1 (en) 1997-02-09

Similar Documents

Publication Publication Date Title
CA1056787A (en) Comminution of solids
US5810266A (en) Process and an apparatus for producing finely divided solids dispersions
US2964382A (en) Production of precipitated calcium carbonate
US5171090A (en) Device and method for dispensing a substance in a liquid
CA1036302A (en) Production of aqueous calcium carbonate suspensions
EP0850685B1 (en) Method of producing dispersed aqueous suspensions
US5342600A (en) Precipitated calcium carbonate
US7169322B2 (en) Aqueous dispersion, process for its production and use
US5160454A (en) Process for manufacturing organoclays having enhanced gelling properties
AU653867B2 (en) A method and arrangement for finely-grinding minerals
US4325514A (en) Comminution of minerals
CA1129753A (en) Predispersed slurry of titanium dioxide
FI973633A (fi) Menetelmä kalsiumkarbonaattipartikkelien valmistamiseksi
US3574135A (en) Production of improved thickened or thixotropic compositions from fluid energy milled colloidal silica
US6451281B1 (en) Methods of manufacturing micro-particulated hydrate slurries
CN1146375A (zh) 氮化硅的自研磨
EP0480587A2 (en) Precipitated calcium carbonate
GB2192558A (en) Emulsifying equipment and method
US5795583A (en) Homogenization of dispersions
CN1039402C (zh) 湿法制备超细重质碳酸钙的方法
US7202197B2 (en) Organic lime slurry and method of preparation
US2658016A (en) Production of fine aqueous dispersion of sulfur
DE69812114D1 (de) Körnige Backhilfe
Yonemoto et al. Continuous synthesis of titanium dioxide fine particles using a slug flow ageing tube reactor
CN1380365A (zh) 涂料生产方法及设备

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C01 Deemed withdrawal of patent application (patent law 1993)
WD01 Invention patent application deemed withdrawn after publication