CN102503500A - In-situ growth titanium carbonitride whisker-toughened silicon nitride-based ceramic tool material and preparation process thereof - Google Patents
In-situ growth titanium carbonitride whisker-toughened silicon nitride-based ceramic tool material and preparation process thereof Download PDFInfo
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- CN102503500A CN102503500A CN2011103617103A CN201110361710A CN102503500A CN 102503500 A CN102503500 A CN 102503500A CN 2011103617103 A CN2011103617103 A CN 2011103617103A CN 201110361710 A CN201110361710 A CN 201110361710A CN 102503500 A CN102503500 A CN 102503500A
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- titanium carbonitride
- silicon nitride
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Abstract
The invention relates to a toughened and reinforced ceramic material and a preparation process thereof, in particular to an in-situ growth titanium carbonitride whisker-toughened silicon nitride-based ceramic tool material and a preparation process thereof. A precursor material for preparing the material comprises the following components in percentage by weight: 25-31 percent of TiO2, 9-12 percent of C, 15-20 percent of NaCl, 15-20 percent of KCl, 1-2 percent of NiCl and the balance of Si3N4. A preparation process comprises the following steps of: mixing a titanium carbonitride-series whisker precursor and silicon nitride particles which are prepared proportionally with absolute ethyl alcohol in a cylinder ball mill by using a stainless steel ball for 24 hours; after uniform mixing, putting a mixture into a vacuum drying oven for drying; after drying, sieving with a 100-mesh sieve; putting obtained composite powder into a graphite container; and synthesizing titanium carbonitride whisker-toughened silicon nitride-based ceramic tool material powder under the condition that the temperature raising rate is 50 DEG C per minute, the flow rate of N2 is 0.1-0.4 Nm<3>/h, the temperature is 1,250-1,500 DEG C, and heat is preserved for 60-120 minutes. The material has the advantages of novel concept, high material quality, various varieties, low cost, simple process, low environment pollution and easiness for industrialization.
Description
One, technical field
The present invention relates to toughened and reinforced stupalith and preparation technology thereof, especially in-situ growth titanium carbonitride crystal whisker toughened ceramice kuife material based on nitrided silicon and preparation technology thereof.
Two, background technology
Structural ceramic material has high firmness, high-wearing feature, high chemical stability and advantage such as high temperature resistant, but stupalith institute inherent fragility has limited its application.The whisker that an amount of interpolation has the higher elasticity modulus can improve the fracture toughness and the bending strength of stupalith greatly.Traditional technology prepares crystal whisker toughened ceramic cutting tool material powder and generally adopts outside mode of adding an amount of whisker and mechanically mixing, and its preparation technology exists that complex process, whisker are prone to that reunion, whisker cost an arm and a leg, contaminate environment and shortcoming such as be detrimental to health.
Patent Office of Intellectual Property in China office is authorized, and the patent No. is " in-situ growth titanium carbonitride crystal whisker toughened aluminum oxide base ceramics cutting tool material powder and the preparation technology thereof " of ZL200610043597.3, with α-Al
2O
3Particle is a matrix; Adding can original position generates the precursor composite powder of whisker; Under suitable growth temperature and soaking time, synthetic alumina base complex phase ceramic powder with certain titanium carbonitride crystal whisker volume content is as the raw material of the crystal whisker toughened ceramic cutting tool material of preparation high-performance then.This patent; Though related to in-situ growth titanium carbonitride crystal whisker; But its titanium carbonitride crystal whisker is single performance kind, and the presoma that generates titanium carbonitride crystal whisker awaits further optimization, and the output of in-situ growth titanium carbonitride crystal whisker and quality and technology all need improve.
Three, summary of the invention
Ti (C
xN
1-x) w is the continuous solid solution that is formed by TiC and TiN, the C atom in the TiC dot matrix can be substituted with any ratio by the N atom, and in like manner, the N atom in the TiN dot matrix can also be substituted with any ratio by the C atom.Ti (C
1-xN
x) performance of w changes with the change of C/N composition to some extent, can play toughened and reinforced effect, therefore can prepare the titanium carbonitride crystal whisker materials.
The objective of the invention is to overcome existing complex phase ceramic powder and preparation technology's thereof defective; Through the carbon titanium nitride crystal whisker that directly growth has plateau modulus in position, silicon nitride matrix Central Plains; For the growth in situ series crystal whisker toughening silicon nitride base ceramic cutting tool material of preparation good mechanical performance provides the complex phase ceramic powdered material and the preparation technology thereof of high-quality, low price, many kinds, add crystal whisker toughened ceramic cutting tool material powder and preparation technology thereof in order to substitute conventional external.
Basic design of the present invention is to be matrix with the silicon nitride particle; Adding can original position generates the precursor composite powder of whisker; Then under suitable growth temperature and soaking time; Synthetic nitride silicon based complex phase ceramic powder with different titanium carbonitride crystal whiskers and certain whisker volume content thereof is as the raw material of the crystal whisker toughened ceramic cutting tool material of preparation high-performance.
In-situ growth titanium carbonitride crystal whisker toughened silicon nitride base ceramic cutting tool material powder, its raw material is by silicon nitride and the precursor powder constituent that can generate titanium carbonitride crystal whisker; Precursor material weight ratio of constituents %:TiO
225%-31%; C 9%-12%; NaCl 15%-20%; KCl 15%-20%; NiCl
21%-2%; Si
3N
4Surplus.
Titanium carbonitride crystal whisker after the generation (containing small quantities of particles) has several, as: TiC
0.1N
0.9, TiC
0.2N
0.8, TiC
0.3N
0.7, TiC
0.5N
0.5, TiC
0.7N
0.3, TiC
0.8N
0.2Deng, the weight content of whisker in nitride silicon based complex phase ceramic powder is: 35%-55%.
The preparation technology of in-situ growth titanium carbonitride crystal whisker toughened silicon nitride base ceramic cutting tool material powder mainly is the whisker in-situ growth technique.This technology is: titanium carbonitride crystal whisker precursor batching and silicon nitride particle that (1) will prepare in proportion add absolute ethyl alcohol and in iar mill, mixed 24 hours with alumina balls; (2) it is dry the compound of mixing to be put into vacuum drying oven, and dry back obtains composite powder with the screening of 100 mesh sieves; (3) composite powder is packed in the crystal vessel, at 50 ℃/min of temperature rise rate, N
2Flow velocity 0.1-0.4Nm
3Under/h, 1250 ℃-1500 ℃ of temperature, the insulation 60min-120min condition, synthetic in-situ grown titanium carbonitride row crystal whisker toughening silicon nitride base ceramic cutting tool material powder.
The present invention is novel, can increase substantially ceramice kuife material based on nitrided silicon fracture toughness and bending strength.Its quality of materials is high, wide in variety, cost is low, and technology is simple, environmental pollution is light, be easy to industrialization.
Four, embodiment:
Pressing composition parameter listed in the embodiment subordinate list forms; Precursor powder thin pulp (adding absolute ethyl alcohol) was mixed 24 hours with alumina balls in iar mill, and it is dry behind the mixing this compound to be put into vacuum drying oven, and screen with 100 mesh sieves dry back; Packing into up and down, sealing, middle top are drilled with in the crystal vessel of aperture; Aperture 3-4mm, girth is 5mm at interval, uniform distribution.Put sintering oven into; Under certain nitrogen flow rate and atmosphere protection thereof (seeing the embodiment subordinate list for details); Under 50 ℃/min of temperature rise rate condition, be warming up to listed temperature in the embodiment parameter subordinate list; Behind the insulation 90min, can obtain the nitride silicon based complex phase ceramic powder of predetermined titanium carbonitride crystal whisker and content, wherein mix small quantities of particles in the titanium carbonitride crystal whisker.
Embodiment parameter subordinate list
* annotate: 1. the TiC in the synthetic powder
xN
1-xMainly form, and mix a spot of particle, 0<x<1 by whisker;
2. experiment statistics shows, titanium carbonitride crystal whisker precursor powder weight sintering rate of loss average out to 73%.
Claims (2)
1. in-situ growth titanium carbonitride crystal whisker toughened ceramice kuife material based on nitrided silicon preparation technology is characterized by precursor material weight ratio of constituents %:TiO
225%-31%; C 9%-12%; NaCl 15%-20%; KCl 15%-20%; NiCl
21%-2%; Si
3N
4Surplus.
2. prepare the described in-situ growth titanium carbonitride crystal whisker toughened ceramice kuife material based on nitrided silicon preparation technology of claim 1; It is characterized by: titanium carbonitride crystal whisker precursor batching and silicon nitride particle that (1) will prepare in proportion add absolute ethyl alcohol and in iar mill, mixed 24 hours with alumina balls; (2) it is dry the compound of mixing to be put into vacuum drying oven, and dry back obtains composite powder with the screening of 100 mesh sieves; (3) composite powder is packed in the crystal vessel, at 50 ℃/min of temperature rise rate, N
2Flow velocity 0.1-0.4Nm
3Under/h, 1250 ℃-1500 ℃ of temperature, the insulation 60min-120min condition, synthetic in-situ grown titanium carbonitride row crystal whisker toughening silicon nitride base ceramic cutting tool material powder.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107829054A (en) * | 2017-11-14 | 2018-03-23 | 湖南大学 | A kind of high-strength tenacity base titanium carbonitride material and preparation method thereof |
CN112479721A (en) * | 2020-10-30 | 2021-03-12 | 江苏材睿科技有限公司 | High-toughness low-resistance silicon nitride ceramic and preparation method thereof |
Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101492306A (en) * | 2009-02-27 | 2009-07-29 | 山东大学 | In situ growth carbon titanium nitride crystal whisker toughening silicon nitride base ceramic cutting tool material powder and producing process thereof |
-
2011
- 2011-11-15 CN CN2011103617103A patent/CN102503500A/en active Pending
Patent Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN101492306A (en) * | 2009-02-27 | 2009-07-29 | 山东大学 | In situ growth carbon titanium nitride crystal whisker toughening silicon nitride base ceramic cutting tool material powder and producing process thereof |
Non-Patent Citations (1)
Title |
---|
蔡志勇: "碳热还原制备Ti(C,N)晶须的研究", 《中国优秀硕士学位论文全文数据库(工程科技I辑)》 * |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107829054A (en) * | 2017-11-14 | 2018-03-23 | 湖南大学 | A kind of high-strength tenacity base titanium carbonitride material and preparation method thereof |
CN107829054B (en) * | 2017-11-14 | 2019-08-30 | 湖南大学 | A kind of high-strength tenacity base titanium carbonitride material and preparation method thereof |
CN112479721A (en) * | 2020-10-30 | 2021-03-12 | 江苏材睿科技有限公司 | High-toughness low-resistance silicon nitride ceramic and preparation method thereof |
CN112479721B (en) * | 2020-10-30 | 2022-07-15 | 江苏材睿科技有限公司 | High-toughness low-resistance silicon nitride ceramic and preparation method thereof |
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Application publication date: 20120620 |