CN1394829A - Microtube titanium carbonate base fibre and its preparation process - Google Patents
Microtube titanium carbonate base fibre and its preparation process Download PDFInfo
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- CN1394829A CN1394829A CN01122724A CN01122724A CN1394829A CN 1394829 A CN1394829 A CN 1394829A CN 01122724 A CN01122724 A CN 01122724A CN 01122724 A CN01122724 A CN 01122724A CN 1394829 A CN1394829 A CN 1394829A
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Abstract
The present invention uses industrial micrometer-grade carbon fiber as raw material, under the action of titanium compound, hydrogen gas and boron or nitride as doping agent and accelerating agent the carbon can be converted into carbide, then the residual carbon is oxidated so as to obtain titanium carbide base hollow tube. It is characterized by that it adopts shape memory method and gas-phase deposition or plasma gas-phase deposition process to make preparation. The internal diameter of the microtube is 0.5-45 micrometer, outer diameter is 5-50 micrometer, volume density is 0.50-2.5g/cu.cm and volume resistance is 0.01-100 ohm.cm. Said material possesses excellent wave-absorbing property, mechanical property and chemical stability.
Description
The invention provides a kind of microtube titanium carbonate base fibre that is used for absorbing material and preparation method thereof.The present invention adopt gas-phase deposition or plasma gas-phase deposit technology with industrial carbon fiber titanizing, then the residual carbon oxidation and product.This material both can be used for structural wave-absorbing material, also can be used for applying absorbing material and anti-microwave lining, and had broad application prospects in fields such as new catalyst, micro sensor, microelectrode, micromechanical component and biomaterials.
Traditional electromagnetic wave absorb mainly contains following several: (1) ultramicro magnetic metal powder and fiber, its subject matter are that the low frequency absorptive character are undesirable, and proportion is bigger.(2) ferrite is widely used in stealthy field.Its main drawback is that density is big, temperature stability is relatively poor.(3), be divided into inorganic loss absorbing material and organic electrical loss absorbing material based on the absorbing material of electrical loss.A focus of inorganic consumable material is the carbon fiber electromagnetic wave absorb, has the characteristics of high-strength light, but high thermal resistance, oxidation-resistance are poor, uses all to plate carbide coating in a lot of occasions.Another focus is the silicon carbide electromagnetic wave absorb, but SiC fiber electrical property belongs to semiconductor material, resistivity is too high, for this reason, attempt by silicon carbide fiber is carried out modification, as regulate its resistivity and change the cross section of fiber, as plate enriched carbon layer, but lost oxidation-resistance, can not deal with problems comprehensively.
At above-mentioned defective, the absorbing material utmost point need be developed the electromagnetic wave absorb with the efficient wave absorbtion in wide territory, high-temperature stability and mechanical property.The present invention takes such scheme: based on the characteristics of the easy titanizing of carbon fiber, with the carbon fiber is raw material, adopt shape memory method and chemical vapor deposition method, under reaction gas titaniferous compound, hydrogen and doping agent and promotor effect as boron or nitrogen compound, carbon fiber is begun to be converted into carbide from the surface, the residual carbon oxidation, get the titanium carbide base open tube then.Because the special property of microtubule electrical conductor, this material electromagnetic parameter can be regulated, and microtexture and size can be controlled, and the absorption of electromagnetic wave performance is better than traditional absorbing material.And this titanium carbide material has advantageous properties such as high rigidity, satisfactory electrical conductivity and thermal conductivity, erosion resistance, resistance to deterioration and high temperature creep-resisting, alternative traditional electromagnetic wave absorb.
The present invention adopts the chemical vapor deposition (CVD) method, is raw material with the micron order carbon fiber, adopts shape memory method and vapour deposition or plasma gas-phase deposit technology, with the rare gas element is carrier gas, under the carrying of hydrogen, feed titaniferous compound gas, under 800-1300 ℃, with H
2Be the carrier gas of titaniferous compound, introduce a small amount of boron or nitrogen compound again, carbon fiber is begun titanizing from the surface,, get the titanium carbide base open tube then with the residual carbon oxidation as doping agent and promotor.Used micron carbon fiber is industry third rare fine base carbon fibre and asphalt base carbon fiber and vapour deposition carbon fiber.Used titaniferous compound is titanium chloride or two luxuriant titaniums, and the nitrogen compound that is adopted is N
2, NH
3, N
2H
4, NF
3Boron compound is BCl
3, BBr
3, B
2H
6
Prepared titanium carbide base tubular fiber microtubule diameter 0.5～45 μ m, external diameter 5～50 μ m adopt different raw materials, control different reaction conditionss, just can obtain different resistivity.Volume density 0.50～2.5g/cm
3, volume specific resistance 0.01～100 Ω cm, anti-corrosion, heatproof, good in oxidation resistance, it is good that mechanics of composites is strengthened property.This inorganic fibre has the absorbing property more superior than tradition, mechanical property, chemical stability and matrix consistency.
Embodiment one
Quality oxide aluminum pipe system horizontal type external-heat reaction tubes, central horizontal is placed aluminum oxide substrate, places raw material PAN base carbon fibre 200mg and a small amount of BCl above
3The saturex evaporating method is adopted in muriatic gasification.Feed unstripped gas from an end of reaction tubes, composed as follows: H
2=50～200sccm, TiCl
4(gas)=10～50sccm carried out vapor deposition reaction 2 hours under 1100 ℃, after the cooling fiber is prescinded, and put into 700 ℃ of calcined oxides of calcining furnace and removed the fibrillar center residual carbon, obtained titanium carbide base tubular fiber microtubule diameter D
1=0.1～0.5 μ m, the microtubule outer diameter D
2=3～5 μ m, volume density 0.50～1.5g/cm
3, volume specific resistance 0.01～1 Ω cm.Fibre chemistry is formed C:41.8～52.5mol%; Ti:45.6～7.9mol%; H:1%～1.4mol%; B:0.3～3.9mol%.
Embodiment two
Quality oxide aluminum pipe system horizontal type external-heat reaction tubes, central horizontal is placed aluminum oxide substrate, places material asphalt base carbon fibre 500mg above.Use the direct current plasma chemical Vapor deposition process.Muriatic gasification saturex evaporating method.Feed unstripped gas from an end of reaction tubes, composed as follows: TiCl
4(gas)=5～100sccm, H
2=20～400sccm, N
2=5～200sccm carried out vapor deposition reaction 3 hours under 1000 ℃, after the cooling fiber is prescinded, and put into 700 ℃ of calcined oxides of calcining furnace and removed the fibrillar center residual carbon, obtained titanium carbide base tubular fiber microtubule diameter D
1=2～5 μ m, the microtubule outer diameter D
2=8～12.5 μ m, volume density 0.50～1.5g/cm
3, volume specific resistance 0.1～10 Ω cm.Fibre chemistry is formed C:43.5～56.2mol%; Ti:42.7～48.9mol%; H:1%～1.4mol%; N:0.9～2.7mol%.
Embodiment three
Quality oxide aluminum pipe system horizontal type external-heat reaction tubes, central horizontal is placed aluminum oxide substrate, places raw material PAN base carbon fibre 500mg above.Feed unstripped gas from an end of reaction tubes, composed as follows: two luxuriant titanium=50sccm, H
2=100sccm, BCl
3=0.5sccm carried out vapor deposition reaction 5 hours under 1050 ℃, after the cooling fiber is prescinded, and put into 800 ℃ of calcined oxides of calcining furnace and removed the fibrillar center residual carbon, obtained titanium carbide base tubular fiber microtubule diameter D
1=1～2 μ m, the microtubule outer diameter D
2=8～12.5 μ m, volume density 0.50～1.5g/cm
3, volume specific resistance 1～10 Ω cm.Fibre chemistry is formed C:45.5～47.4mol%; Ti:46.9～48.8mol%; H:1%～1.4mol%; B:0.1～2.9mol%.
Claims (2)
1. microtube titanium carbonate base fibre and preparation method thereof, with industrial micron order carbon fiber is raw material, under reaction gas effects such as titaniferous compound and hydrogen carbon is converted into carbide, its characteristics are: adopt shape memory method and vapour deposition or plasma gas-phase deposit prepared micron order tubulose TiC base fiber; Its microtubule diameter 0.5～45 μ m, external diameter 5～50 μ m, volume density 0.50～2.5g/cm
3, volume specific resistance 0.01～100 Ω cm.
2. microtube titanium carbonate base fibre according to claim 1 and preparation method thereof, its characteristics are: in reaction process, introducing titaniferous compound and a small amount of compound boron or nitrogen compound is doping agent and promotor, carbon fiber is begun to be converted into the doping titanium carbide from the surface, the residual carbon oxidation, get the titanium carbide base open tube then.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN01122724A CN1394829A (en) | 2001-07-11 | 2001-07-11 | Microtube titanium carbonate base fibre and its preparation process |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN01122724A CN1394829A (en) | 2001-07-11 | 2001-07-11 | Microtube titanium carbonate base fibre and its preparation process |
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| CN1394829A true CN1394829A (en) | 2003-02-05 |
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| CN01122724A Pending CN1394829A (en) | 2001-07-11 | 2001-07-11 | Microtube titanium carbonate base fibre and its preparation process |
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|---|---|---|---|---|
| CN101838501A (en) * | 2010-05-26 | 2010-09-22 | 福建泉州市建田漆业有限公司 | Oily antiradar coating and preparation method thereof |
| CN101857758A (en) * | 2010-05-26 | 2010-10-13 | 福建泉州市建田漆业有限公司 | Aqueous wave absorbing coating and preparation method thereof |
| US10696553B2 (en) | 2014-03-21 | 2020-06-30 | Ford Global Technologies, Llc | Method of forming carbon fibers having internal cavities |
| US11444397B2 (en) | 2015-07-07 | 2022-09-13 | Amphenol Fci Asia Pte. Ltd. | Electrical connector with cavity between terminals |
| US11469553B2 (en) | 2020-01-27 | 2022-10-11 | Fci Usa Llc | High speed connector |
| US11522310B2 (en) | 2012-08-22 | 2022-12-06 | Amphenol Corporation | High-frequency electrical connector |
| US11539171B2 (en) | 2016-08-23 | 2022-12-27 | Amphenol Corporation | Connector configurable for high performance |
| US11715914B2 (en) | 2014-01-22 | 2023-08-01 | Amphenol Corporation | High speed, high density electrical connector with shielded signal paths |
| US11757224B2 (en) | 2010-05-07 | 2023-09-12 | Amphenol Corporation | High performance cable connector |
| US11757215B2 (en) | 2018-09-26 | 2023-09-12 | Amphenol East Asia Electronic Technology (Shenzhen) Co., Ltd. | High speed electrical connector and printed circuit board thereof |
| US11799246B2 (en) | 2020-01-27 | 2023-10-24 | Fci Usa Llc | High speed connector |
| US11817655B2 (en) | 2020-09-25 | 2023-11-14 | Amphenol Commercial Products (Chengdu) Co., Ltd. | Compact, high speed electrical connector |
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-
2001
- 2001-07-11 CN CN01122724A patent/CN1394829A/en active Pending
Cited By (19)
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|---|---|---|---|---|
| US11757224B2 (en) | 2010-05-07 | 2023-09-12 | Amphenol Corporation | High performance cable connector |
| CN101857758A (en) * | 2010-05-26 | 2010-10-13 | 福建泉州市建田漆业有限公司 | Aqueous wave absorbing coating and preparation method thereof |
| CN101838501B (en) * | 2010-05-26 | 2013-02-06 | 福建泉州市建田漆业有限公司 | Oily antiradar coating and preparation method thereof |
| CN101857758B (en) * | 2010-05-26 | 2013-04-24 | 福建泉州市建田漆业有限公司 | Aqueous wave absorbing coating and preparation method thereof |
| CN101838501A (en) * | 2010-05-26 | 2010-09-22 | 福建泉州市建田漆业有限公司 | Oily antiradar coating and preparation method thereof |
| US11522310B2 (en) | 2012-08-22 | 2022-12-06 | Amphenol Corporation | High-frequency electrical connector |
| US11901663B2 (en) | 2012-08-22 | 2024-02-13 | Amphenol Corporation | High-frequency electrical connector |
| US11715914B2 (en) | 2014-01-22 | 2023-08-01 | Amphenol Corporation | High speed, high density electrical connector with shielded signal paths |
| US10696553B2 (en) | 2014-03-21 | 2020-06-30 | Ford Global Technologies, Llc | Method of forming carbon fibers having internal cavities |
| US11444397B2 (en) | 2015-07-07 | 2022-09-13 | Amphenol Fci Asia Pte. Ltd. | Electrical connector with cavity between terminals |
| US11955742B2 (en) | 2015-07-07 | 2024-04-09 | Amphenol Fci Asia Pte. Ltd. | Electrical connector with cavity between terminals |
| US11539171B2 (en) | 2016-08-23 | 2022-12-27 | Amphenol Corporation | Connector configurable for high performance |
| US11757215B2 (en) | 2018-09-26 | 2023-09-12 | Amphenol East Asia Electronic Technology (Shenzhen) Co., Ltd. | High speed electrical connector and printed circuit board thereof |
| US11469554B2 (en) | 2020-01-27 | 2022-10-11 | Fci Usa Llc | High speed, high density direct mate orthogonal connector |
| US11469553B2 (en) | 2020-01-27 | 2022-10-11 | Fci Usa Llc | High speed connector |
| US11799246B2 (en) | 2020-01-27 | 2023-10-24 | Fci Usa Llc | High speed connector |
| US11817657B2 (en) | 2020-01-27 | 2023-11-14 | Fci Usa Llc | High speed, high density direct mate orthogonal connector |
| US11942716B2 (en) | 2020-09-22 | 2024-03-26 | Amphenol Commercial Products (Chengdu) Co., Ltd. | High speed electrical connector |
| US11817655B2 (en) | 2020-09-25 | 2023-11-14 | Amphenol Commercial Products (Chengdu) Co., Ltd. | Compact, high speed electrical connector |
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