CN101870592A - Preparation method of titanium-nitride silicon carbide fibers - Google Patents
Preparation method of titanium-nitride silicon carbide fibers Download PDFInfo
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- CN101870592A CN101870592A CN 201010213624 CN201010213624A CN101870592A CN 101870592 A CN101870592 A CN 101870592A CN 201010213624 CN201010213624 CN 201010213624 CN 201010213624 A CN201010213624 A CN 201010213624A CN 101870592 A CN101870592 A CN 101870592A
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Abstract
The invention relates to a preparation method of titanium-nitride silicon carbide fibers, which is characterized by comprising the following steps of: firstly, selecting alcohol based on the mass ratio: 1 percent of silicon carbide fibers and 6 percent of metal titanium power and the proportion: 5-6g of the silicon carbide fibers and 150mL of the alcohol, adding the alcohol after mixing the silicon carbide fibers and the metal titanium power, and obtaining mixed power A by wet grinding the mixture; secondly, selecting hydrochloride based on the proportion: 5-6g of the silicon carbide fibers and 30mL of the hydrochloride, selecting acetone based on the volume ratio: 2 percent of the hydrochloride and 10-15 percent of the acetone, and obtaining a mixed solution by mixing the hydrochloride and the acetone; thirdly, obtaining a suspension solution by ultrasonically dispersing the mixed power A after wet grinding in the mixed solution; fourthly, vacuum drying; fifthly, obtaining mixed power C through microwave heating treatment under the protection of nitrogen; and sixthly, obtaining the titanium-nitride silicon carbide fibers by sieving the mixed power C through a 200-mesh sieve. The invention has the advantages of low cost, simple process, easy control and scale production.
Description
Technical field
The present invention relates to a kind of preparation method of silicon carbide fiber.
Background technology
Silicon carbide claims moissanite again.In non-oxidized substance hi-tech refractory raw materials such as contemporary C, N, B, silicon carbide is most widely used general, most economical a kind of.Can be called powder emery or fire sand.Silicon carbide fiber because of its stable chemical performance, thermal expansivity is little, wear resisting property good, thermotolerance and scale resistance all are better than carbon fiber, intensity reaches advantages such as 1960～4410MPa, obtained using widely (Th.Schubert, et al.Mater.Sci.Eng., A, 475 (2008) 39-44).Silicon carbide fiber is to be that raw material makes the inorganic fibre with silicon B-carbide structure through spinning, carbonization or vapour deposition with silicoorganic compound, belongs to the ceramic fiber class.Continuous fibre is that silicon carbide is coated on the core silks such as tungsten filament or carbon fiber and the continuous fibers that form or spinning and pyrolysis and obtain the pure carbon silicon filament.
Common silicon carbide fiber is owing to contain more Si
xC
yO
zPhase sharply descends intensity taking place easily more than 1200 ℃ to decompose; Fast development along with silicon carbide fiber research, obtained very big progress in high temperature resistant technical field, Japan carbon company adopts electron radiation to replace conventional air preoxidation, thereby reduced the oxygen level in the fiber very significantly, the use temperature of the Hi-Nicalon fiber of being produced can reach 1400 ℃ of (H.P.Baldus, et al.Jansen.Angew.Chem.Int.Ed., 36 (1997) 328-333).But this method cost is very high.The method for preparing the most economical practicality of high temperature resistant SiC fiber is to introduce a small amount of different element in the precursor of SiC fiber, plays the effect of sintering aid, carries out high temperature deoxidation sintering processes again.U.S. Sylramic and Japanese Tyranno SA fiber are the superhigh temperature resistant SiC fibers of introducing a certain amount of sintering aid B and Al in preparation process respectively.Company of Ube Industries Ltd. introduces boron and suppresses silicon carbide fiber crystallization at high temperature in the precursor Polycarbosilane (PCS) of silicon carbide fiber, make the use temperature of fiber bring up to (K.Kumagawa about 1500 ℃, et al.Ceram.Eng.Sci.Proc., 1998,19 (3) 65-72).
Mainly as high temperature material and strongthener, high temperature material comprises the filter cloth of heatshield material, high temperature-resistance conveyor belt, filtration high-temperature gas or molten metal etc. to silicon carbide fiber.When being used as strongthener, normal and carbon fiber or glass fibre share, to strengthen metal (as aluminium) and ceramic main, as make brake facing, engine blade, landing wheel casing and the airframe material etc. of jet plane, also can be used as sports goods, its chopped strand then can be used as High Temperature Furnaces Heating Apparatus material etc.Silicon carbide fiber obtains comparatively extensive studies (X.Luo, et al.Scripta Mater., 56 (2007) 569-572s) as strengthening toughening material because of its excellent physical chemistry and mechanical property in copper base heat sink material.But silicon carbide fiber is in the process of synthetic copper based composite metal material, and maximum problem is that surface reaction takes place, reaction produces thermal conductance and the specific conductivity (X.Luo that the Si element will reduce matrix material greatly, et al.Mater.Sci.Eng., A, 459 (2007) 244-250).In order to reduce surface reaction as far as possible, available metal coating stops copper and silicon carbide generation surface reaction, for example: electroplated Ni coating (X.Luo, et al.J.Alloys Compd., 469 (2009) 237-243), vapour deposition Mo coating (Th.Schubert, et al.CompositesPart A, 38 (2007) 2398-2403), magnetron sputtering Ti coating (A.Brende l, et al.Surf.Coat.Techno 1., 200 (2005) 161-164), magnetron sputtering C r and W coating (T.
Et al.J.Nucl.Mater., 362 (2007) 197-201) and laser cladding Fe-Cr-Mo layer (A.Basu, et al.Surf.Coat.Technol., 202 (2008) 2623-2631) etc.At present, about using more sophisticated method in the method for titanizing the little evaporation titanizing of vacuum technology is arranged, be mainly used in diamond surface metallization, can improve adamantine thermostability greatly, the defective of diamond surface is made up, crack tip passivation (Wang Yanhui etc., diamond and grinding materials and grinding tool engineering, 169 (2009) 5-8).The major advantage of this method is advantages (Li Guobin etc., diamond and grinding materials and grinding tool engineering, 158 (2007) 14-19) such as the plating quality is higher, single plating amount is big, but high vacuum condition is relatively harsher, equipment is relatively costly.Required equipment, sputtering condition and the parameter of another kind of commonly used magnetron sputtering titanizing method is also relatively complicated, the production cost height, is difficult for producing in enormous quantities.
Summary of the invention
The purpose of this invention is to provide that a kind of cost is low, technology simply, the preparation method of the titanium-nitride silicon carbide fibers of control and large-scale production easily.
In order to realize purpose of the present invention, technical scheme of the present invention is: the preparation method of titanium-nitride silicon carbide fibers is characterized in that it comprises the steps:
1) press silicon carbide fiber: the mass ratio of metallic titanium powder=1: 6, take by weighing silicon carbide fiber and metallic titanium powder, press silicon carbide fiber: the proportioning of alcohol=5～6g: 150mL, choose alcohol, standby; Wherein the diameter of silicon carbide fiber is about 14 μ m, length is 5～15mm, and the granularity of metallic titanium powder is 300～400 orders;
Silicon carbide fiber and metallic titanium powder are mixed the wet-milling of back adding alcohol, obtain mixed powder A;
2) press silicon carbide fiber: the proportioning=5～6g of hydrochloric acid (HCl): 30mL, choose hydrochloric acid; Press hydrochloric acid: acetone (CH
3COCH
3) volume ratio=2: 10～15, choose acetone; Hydrochloric acid is mixed with acetone, obtain mixing solutions;
3) mixed powder A that wet-milling is good ultra-sonic dispersion 5～10 minutes in mixing solutions, violent stirring is 10～20 minutes then, obtains suspension solution;
4) suspension solution filters, after the removal filtrate, and vacuum-drying, drying temperature is 50～70 ℃, obtains pretreated mixed powder B;
5) microwave heating treatment under the nitrogen protection: pretreated mixed powder B is put into alumina crucible, place microwave sintering device cavity, under the nitrogen protection environment, carry out coating film treatment, be warmed up to 800～1000 ℃ with 50～200 ℃/minute of temperature rise rates, be incubated 5～20 minutes, after treating that furnace temperature is reduced to room temperature, take out alumina crucible, obtain mixed powder C;
6) with mixed powder C through 200 purpose sieve after, obtain titanium-nitride silicon carbide fibers.
Described ultrasound condition: power is 60～100W, and frequency is 20～40KHz.
Described violent stirring is meant that rotating speed is more than 500 rev/mins.
Described microwave heating treatment processing condition: microwave frequency is 2.45GHz, and power is 0.5～4KW.
The invention has the beneficial effects as follows:
1, cost is low: the starting material component that uses in the preparation process is few, and technology is simple, equipment is simple, therefore has the low characteristics of cost.
2, the preparation process processing step is few, and required equipment is simple, has made full use of the characteristics of microwave sintering process; Therefore have that generated time is short, technology simply, the characteristics of control and large-scale production easily.
3, its titanium film densification of the titanium-nitride silicon carbide fibers that obtains can be widely used in strengthening materials such as toughness reinforcing heat sink material.
Description of drawings
Fig. 1 is preparation technology's schema of the present invention;
Fig. 2 is the X ray diffracting spectrum that the original silicon carbide fiber and the embodiment of the invention 1 make titanium-nitride silicon carbide fibers;
Fig. 3 a is the sem photograph of original silicon carbide fiber;
Fig. 3 b is the enlarged view of Fig. 3 a;
Fig. 4 a is the sem photograph that example 1 of the present invention makes titanium-nitride silicon carbide fibers;
Fig. 4 b is the enlarged view of Fig. 4 a.
Embodiment
Further the present invention will be described below in conjunction with drawings and Examples, but that content of the present invention not only is confined to is following
Embodiment.
Embodiment 1:
As shown in Figure 1, the preparation method of titanium-nitride silicon carbide fibers, it comprises the steps:
1) (diameter is about 14 μ m, length and is about 5～15mm) and 30g, about 400 order metallic titanium powder, adds the alcohol wet-milling of 150mL, obtains mixed powder A to take by weighing the silicon carbide fiber of 5g; 2) measure 30mL hydrochloric acid, 150mL acetone, be configured to mixing solutions; 3) with mixed powder A ultra-sonic dispersion 5 minutes in mixing solutions, continue violent stirring then 10 minutes, obtain suspension solution; 4) suspension solution filters back (removing filtrate), vacuum-drying, and drying temperature is 50 ℃, obtains pretreated mixed powder B; 5) pretreated mixed powder B is put into alumina crucible, place microwave sintering device cavity, under the nitrogen protection environment, carry out coating film treatment, the frequency of using is at 2.45GHz, and power is controlled at 4KW, is warmed up to 1000 ℃ with 200 ℃/minute of temperature rise rates, be incubated 5 minutes, after treating that furnace temperature is reduced to room temperature, take out alumina crucible, obtain mixed powder C; 6) with mixed powder C through 200 purpose sieve after, obtain titanium-nitride silicon carbide fibers.
Fig. 2 is the X ray diffracting spectrum of titanium-nitride silicon carbide fibers, shows to adopt this titanium-nitride technology to coat titanium nitride film on the silicon carbide fiber surface.Fig. 3 (a) is the sem photograph of original silicon carbide fiber, and Fig. 3 (b) is its enlarged view.Fig. 4 (a) is the sem photograph of the silicon carbide fiber after the titanium-nitride, and Fig. 4 (b) be the partial enlarged drawing of titanium-nitride silicon carbide fibers, shown silicon carbide plating one deck titanium nitride film, surfaces nitrided titanium layer densification, even.
Embodiment 2:
As shown in Figure 1, the preparation method of titanium-nitride silicon carbide fibers, it comprises the steps:
1) (diameter is about 14 μ m, length and is about 5～15mm) and 36g, about 300 order metallic titanium powder, adds the alcohol wet-milling of 150mL, obtains mixed powder A to take by weighing the silicon carbide fiber of 6g; 2) measure 30mL hydrochloric acid, 225mL acetone, be configured to mixing solutions; 3) with mixed powder A ultra-sonic dispersion 10 minutes in mixing solutions, continue violent stirring then 20 minutes, obtain suspension solution; 4) suspension solution filters back (removing filtrate), vacuum-drying, and drying temperature is 70 ℃, obtains pretreated mixed powder B; 5) pretreated mixed powder B is put into alumina crucible, place microwave sintering device cavity, under the nitrogen protection environment, carry out coating film treatment, the frequency of using is at 2.45GHz, and power is controlled at 0.5KW, is warmed up to 800 ℃ with 50 ℃/minute of temperature rise rates, be incubated 20 minutes, after treating that furnace temperature is reduced to room temperature, take out alumina crucible, obtain mixed powder C; 6) with mixed powder C through 200 purpose sieve after, obtain titanium-nitride silicon carbide fibers.
Embodiment 3:
As shown in Figure 1, the preparation method of titanium-nitride silicon carbide fibers, it comprises the steps:
1) (diameter is about 14 μ m, length and is about 5～15mm) and 36g, about 400 order metallic titanium powder, adds the alcohol wet-milling of 150mL, obtains mixed powder A to take by weighing the silicon carbide fiber of 6g; 2) measure 30mL hydrochloric acid, 200mL acetone, be configured to mixing solutions; 3) with mixed powder A ultra-sonic dispersion 8 minutes in mixing solutions, continue violent stirring then 15 minutes, obtain suspension solution; 4) suspension solution filters back (removing filtrate), vacuum-drying, and drying temperature is 60 ℃, obtains pretreated mixed powder B; 5) pretreated mixed powder B is put into alumina crucible, place microwave sintering device cavity, under the nitrogen protection environment, carry out coating film treatment, the frequency of using is at 2.45GHz, and power is controlled at 2.5KW, is warmed up to 900 ℃ with 100 ℃/minute of temperature rise rates, be incubated 15 minutes, after treating that furnace temperature is reduced to room temperature, take out alumina crucible, obtain mixed powder C; 6) with mixed powder C through 200 purpose sieve after, obtain titanium-nitride silicon carbide fibers.
Embodiment 4:
As shown in Figure 1, the preparation method of titanium-nitride silicon carbide fibers, it comprises the steps:
1) (diameter is about 14 μ m, length and is about 5～15mm) and 30g, 300 order metallic titanium powder, adds the alcohol wet-milling of 150mL, obtains mixed powder A to take by weighing the silicon carbide fiber of 5g; 2) measure 30mL hydrochloric acid, 180mL acetone, be configured to mixing solutions; 3) with mixed powder A ultra-sonic dispersion 8 minutes in mixing solutions, continue violent stirring then 20 minutes, obtain suspension solution; 4) suspension solution filters back (removing filtrate), vacuum-drying, and drying temperature is 65 ℃, obtains pretreated mixed powder B; 5) pretreated mixed powder B is put into alumina crucible, place microwave sintering device cavity, under the nitrogen protection environment, carry out coating film treatment, the frequency of using is at 2.45GHz, and power is controlled at 3.0KW, is warmed up to 850 ℃ with 150 ℃/minute of temperature rise rates, be incubated 18 minutes, after treating that furnace temperature is reduced to room temperature, take out alumina crucible, obtain mixed powder C; 6) with mixed powder C through 200 purpose sieve after, obtain titanium-nitride silicon carbide fibers.
Each cited raw material of the present invention can both be realized the present invention, and the bound value of each raw material, interval value can both realize the present invention, the bound value and the interval value of processing parameter of the present invention (as temperature, time, vacuum tightness etc.) can both be realized the present invention, do not enumerate embodiment one by one at this.
Claims (3)
1. the preparation method of titanium-nitride silicon carbide fibers is characterized in that it comprises the steps:
1) press silicon carbide fiber: the mass ratio of metallic titanium powder=1: 6, take by weighing silicon carbide fiber and metallic titanium powder, press silicon carbide fiber: the proportioning of alcohol=5～6g: 150mL, choose alcohol, standby; Silicon carbide fiber and metallic titanium powder are mixed the wet-milling of back adding alcohol, obtain mixed powder A;
2) press silicon carbide fiber: the proportioning of hydrochloric acid=5～6g: 30mL, choose hydrochloric acid; Press hydrochloric acid: the volume ratio of acetone=2: 10～15, choose acetone; Hydrochloric acid is mixed with acetone, obtain mixing solutions;
3) mixed powder A that wet-milling is good ultra-sonic dispersion 5～10 minutes in mixing solutions, violent stirring is 10～20 minutes then, obtains suspension solution;
4) suspension solution filters, after the removal filtrate, and vacuum-drying, drying temperature is 50～70 ℃, obtains pretreated mixed powder B;
5) microwave heating treatment under the nitrogen protection: pretreated mixed powder B is put into alumina crucible, place microwave sintering device cavity, under the nitrogen protection environment, carry out coating film treatment, be warmed up to 800～1000 ℃ with 50～200 ℃/minute of temperature rise rates, be incubated 5～20 minutes, after treating that furnace temperature is reduced to room temperature, take out alumina crucible, obtain mixed powder C;
6) with mixed powder C through 200 purpose sieve after, obtain titanium-nitride silicon carbide fibers.
2. the preparation method of titanium-nitride silicon carbide fibers according to claim 1, it is characterized in that: the diameter of described silicon carbide fiber is that 14 μ m, length are 5～15mm.
3. the preparation method of titanium-nitride silicon carbide fibers according to claim 1, it is characterized in that: the granularity of described metallic titanium powder is 300～400 orders.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103409732A (en) * | 2013-07-25 | 2013-11-27 | 西南石油大学 | Composite processing method for realizing metallization of surfaces of diamonds |
| CN105200759A (en) * | 2015-09-05 | 2015-12-30 | 苏州宏久航空防热材料科技有限公司 | Preparation method of short cut silicon carbide fiber with aluminum oxide structure surface layer |
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| US5082810A (en) * | 1990-02-28 | 1992-01-21 | E. I. Du Pont De Nemours And Company | Ceramic dielectric composition and method for preparation |
| CN1854105A (en) * | 2004-12-31 | 2006-11-01 | 电子科技大学 | Nanometer ceramic-material doping agent, ceramic capacitor media material and production thereof |
| WO2007039310A1 (en) * | 2005-10-06 | 2007-04-12 | Vesuvius Crucible Company | Crucible for the crystallization of silicon and process for making the same |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02296764A (en) * | 1989-05-12 | 1990-12-07 | Nkk Corp | Production of porcelain |
| US5082810A (en) * | 1990-02-28 | 1992-01-21 | E. I. Du Pont De Nemours And Company | Ceramic dielectric composition and method for preparation |
| CN1854105A (en) * | 2004-12-31 | 2006-11-01 | 电子科技大学 | Nanometer ceramic-material doping agent, ceramic capacitor media material and production thereof |
| WO2007039310A1 (en) * | 2005-10-06 | 2007-04-12 | Vesuvius Crucible Company | Crucible for the crystallization of silicon and process for making the same |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103409732A (en) * | 2013-07-25 | 2013-11-27 | 西南石油大学 | Composite processing method for realizing metallization of surfaces of diamonds |
| CN103409732B (en) * | 2013-07-25 | 2015-11-04 | 西南石油大学 | A kind of compounding method of diamond surface metallization |
| CN105200759A (en) * | 2015-09-05 | 2015-12-30 | 苏州宏久航空防热材料科技有限公司 | Preparation method of short cut silicon carbide fiber with aluminum oxide structure surface layer |
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