CN108191443A - A kind of chopped strand enhances three silication, five titanium composite material preparation method - Google Patents

A kind of chopped strand enhances three silication, five titanium composite material preparation method Download PDF

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Publication number
CN108191443A
CN108191443A CN201711325367.0A CN201711325367A CN108191443A CN 108191443 A CN108191443 A CN 108191443A CN 201711325367 A CN201711325367 A CN 201711325367A CN 108191443 A CN108191443 A CN 108191443A
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powder
ball
abrading
silication
fiber
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方双全
秦云晴
黄新
田郭涛
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Yangzhou University
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Yangzhou University
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    • 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
    • C04B35/58085—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 silicides
    • C04B35/58092—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 silicides based on refractory metal silicides
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    • 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
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    • 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
    • C04B35/62615—High energy or reactive ball milling
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    • 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
    • C04B35/64—Burning or sintering processes
    • C04B35/645—Pressure sintering
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/658—Atmosphere during thermal treatment
    • C04B2235/6581—Total pressure below 1 atmosphere, e.g. vacuum

Abstract

The present invention relates to a kind of chopped strands to enhance three silication, five titanium composite material preparation method.The present invention weighs Si powder with Ti powder as mechanical alloying raw material at 3: 5 in molar ratio, using ZrO2For Ceramic Balls as abrading-ball, the mass ratio of abrading-ball and raw material is 10 20: 1, measures the process control agent of 0.1 0.3 times of ball milling tank volumes, adds in ball grinder, and using Ar gas as protective gas, vacuum drying is ground, and obtains Ti5Si3Powder, with hydrochloric acid to obtained Ti5Si3Powder is handled, by fiber and Ti5Si3Powder is mixed, vacuum drying, by Ti5Si3Fiber composite powder, which is put into graphite jig, is warming up to 1400 DEG C, and furnace cooling to room temperature obtains Fiber Reinforced Ti5Si3Based composites.The present invention overcomes the defects of complex technical process or high price.The simple and reliable easy realization of the present invention, and the Ti prepared5Si3Based composites, consistency is high, the porosity is small, purity is high, excellent in mechanical performance.

Description

A kind of chopped strand enhances three silication, five titanium composite material preparation method
Technical field
The present invention relates to a kind of fibre reinforced composites, more particularly to a kind of chopped strand enhancing three silication, five titanium Composite material and preparation method thereof.
Background technology
Ti5Si3It is a kind of potential high-temperature structural material for being used for 1600 DEG C or more, but Room-Temperature Fracture Toughness is low, high temperature is strong Spend the characteristics of not high enough restricts its application in practical field always.
Before the present invention makes, at present to Ti5Si3The method of intermetallic compound Strengthening and Toughening mainly has crystal grain thinning, closes Aurification and Composite method.It can be changed using crystal grain refinement and adjust heterogeneous microstructure, carry out plasticity secondary phase toughening, led to The reciprocation of crackle and Plastic phase is crossed to increase toughness, but effect is not very significantly.Alloying is in Ti5Si3Middle addition is resistance to Thermometal element forms solid solution to improve its performance, but these elements at high temperature cannot and Ti5Si3Complete chemical compatibility, and And increase Ti5Si3Density；It adds the reinforced phases such as ceramic particle, fiber or whisker and prepares Ti5Si3Based composites are mesh The preceding most common approach for improving mechanical property.But some reinforced phases only serve toughening effect, and intensity is not influenced；It is and another Low-alloyed intensity also even drops while toughening a bit.It is well known that it is simple for process to add rigid ceramic particle, but toughening Effect unobvious；The strength and toughness of intermetallic compound, but complex technical process can be effectively improved using continuous fiber；It is brilliant Must Strengthening and Toughening intermetallic compound significant effect, it is and simple for process, but the price limit of whisker costliness its in practical field In application.
Invention content
The purpose of the present invention, which is that, overcomes drawbacks described above, provides a kind of chopped strand enhancing three silication, five titanium composite material Preparation method.
The technical scheme is that：
A kind of chopped strand enhances three silication, five titanium composite material preparation method, is mainly characterized by step such as Under：
(1) Si powder is weighed with Ti powder as mechanical alloying raw material at 3: 5 in molar ratio；
(2) using ZrO2For Ceramic Balls as abrading-ball, the mass ratio of abrading-ball and raw material is 10-20: 1；
(3) process control agent of 0.1-0.3 times of ball milling tank volume is measured；
(4) raw material, abrading-ball together with process control agent are added in into ball grinder, using Ar gas as protective gas, will be sealed Ball grinder be put into high-energy planetary ball mill machine and rotate；
(5) gained ball milling powder is dried in vacuo, ground, crossed 130 mesh sieve and obtain Ti5Si3Powder；
(6) chopped strand is surface-treated with surfactant, with hydrochloric acid to obtained Ti5Si3At powder Reason, by the fiber handled well and Ti5Si3Powder is mixed；
(7) it is dried in vacuo, obtains Ti5Si3Fiber composite powder；
(8) by Ti5Si3Fiber composite powder is put into graphite jig, is put into vacuum degree less than 1.0 × 10-2Vacuum hotpressing In stove, 1400 DEG C are warming up to, furnace cooling to room temperature obtains Fiber Reinforced Ti5Si3Based composites.
Setting speed is 300-500 revs/min in the step (4), and Ball-milling Time is 10-50 hours.
The vacuum degree of vacuum hotpressing stove is less than 1.0 × 10 in the step (8), and 1400 are warming up to the speed of 10 DEG C/min DEG C, 120 minutes are kept the temperature, maximum pressure 30MPa.
The simple and reliable easy realization of the present invention, uses sub-micron, nano level silica flour and titanium valve as raw material, has excellent mechanical Performance and high temperature resistant chopped strand are as reinforcing agent, using mechanical alloying, ultrasonic disperse and vacuum hot-pressed sintered technology, so as to Prepare the Fiber Reinforced Ti of excellent in mechanical performance5Si3Based composites, and Ti5Si3Based composites, consistency is high, stomata Rate is small, purity is high, excellent in mechanical performance.
Specific embodiment
1st, Si powder and Ti powder are weighed as mechanical alloying raw material at 3: 5 in molar ratio；Using various sizes of ZrO2Ceramics For ball as abrading-ball, abrading-ball large-sized in this way generates percussion to material, plays the role of fragmentation material, the material of fragmentation into Enter to globular spaces of Czermak, by further levigate.The mass ratio of abrading-ball and raw material is 10-20: 1；Measure 0.1-0.3 times of ball milling tank volume Process control agent；Raw material, abrading-ball together with process control agent are added in into ball grinder, using Ar gas as protective gas, will be sealed Good ball grinder is put into high-energy planetary ball mill machine, and setting speed is 300-500 revs/min, and Ball-milling Time is 10-50 hours； Gained ball milling powder is dried in vacuo, is ground, 130 mesh sieve is crossed and obtains Ti5Si3Powder.Used process control agent is four Chlorination carbon, it is good not only to go out powder effect, nor oxidizing fire phenomenon occurs；
2nd, fiber is surface-treated using appropriate surfactant, using hydrochloric acid to obtained Ti5Si3Powder into Row processing, then by the fiber handled well and Ti5Si3Powder is mixed, and homodisperse, Ran Houjin is realized using ultrasonic wave Row vacuum drying, obtains Ti5Si3Fiber composite powder.
3rd, in order to improve the consistency of sintered body, first by composite powder cold isostatic compaction, green compact is then put into stone In black mold, then vacuum degree is placed in less than 1.0 × 10-2In vacuum hotpressing stove, 1400 DEG C are warming up to the speed of 10 DEG C/min, is protected Temperature 120 minutes.Maximum pressure is 30MPa, and furnace cooling to room temperature obtains Fiber Reinforced Ti5Si3Based composites.
Embodiment：
20% chopped carbon fiber enhances Ti5Si3The preparation of composite material.Weigh Si powder with Ti powder as machine at 3: 5 in molar ratio Tool alloyed feedstock；Using various sizes of ZrO2For Ceramic Balls as abrading-ball, the mass ratio of abrading-ball and raw material is 20: 1；It measures The process control agent of 0.23 times of ball milling tank volume；Raw material, abrading-ball are added in into ball grinder together with process control agent, using Ar gas as The ball grinder being sealed is put into high-energy planetary ball mill machine by protective gas, and setting speed is 450 revs/min, and Ball-milling Time is 40 hours；Gained ball milling powder is dried in vacuo, is ground, 130 mesh sieve is crossed and obtains Ti5Si3Powder.Utilize dodecyl sulphur Sour sodium is surface-treated carbon fiber, then the Ti with being crossed with HCl treatment as surfactant5Si3Powder carries out ultrasound Dispersion, drying, obtain 20% fibre reinforced Ti5Si3Composite powder, then vacuum heating-press sintering is carried out, carbon fiber increasing is prepared Strong Ti5Si3Composite material.

Claims (3)

1. a kind of chopped strand enhances three silication, five titanium composite material preparation method, it is characterised in that step is as follows：
(1) Si powder is weighed with Ti powder as mechanical alloying raw material at 3: 5 in molar ratio；
(2) using ZrO2For Ceramic Balls as abrading-ball, the mass ratio of abrading-ball and raw material is 10-20: 1；
(3) process control agent of 0.1-0.3 times of ball milling tank volume is measured；
(4) raw material, abrading-ball are added in into ball grinder together with process control agent, using Ar gas as protective gas, the ball that will be sealed Grinding jar, which is put into high-energy planetary ball mill machine, to be rotated；
(5) gained ball milling powder is dried in vacuo, ground, crossed 130 mesh sieve and obtain Ti5Si3Powder；
(6) chopped strand is surface-treated with surfactant, with hydrochloric acid to obtained Ti5Si3Powder is handled, will The fiber and Ti handled well5Si3Powder is mixed；
(7) it is dried in vacuo, obtains Ti5Si3Fiber composite powder；
(8) by Ti5Si3Fiber composite powder is put into graphite jig, is put into vacuum degree less than 1.0 × 10-2In vacuum hotpressing stove, 1400 DEG C are warming up to, furnace cooling to room temperature obtains Fiber Reinforced Ti5Si3Based composites.
2. a kind of chopped strand enhancing three silication, five titanium composite material preparation method according to claim 1, feature exist Setting speed is 300-500 revs/min in the step (4), and Ball-milling Time is 10-50 hours.
3. a kind of chopped strand enhancing three silication, five titanium composite material preparation method according to claim 1, feature exist The vacuum degree of vacuum hotpressing stove is less than 1.0 × 10 in the step (8)-2, 1400 DEG C are warming up to the speed of 10 DEG C/min, is protected Temperature 120 minutes, maximum pressure 30MPa.
CN201711325367.0A 2017-12-08 2017-12-08 A kind of chopped strand enhances three silication, five titanium composite material preparation method Pending CN108191443A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114560713A (en) * 2022-03-01 2022-05-31 北京科技大学 Preparation method of carbon fiber toughened Ti-Si-C intermetallic compound composite material

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JPH04119967A (en) * 1990-09-11 1992-04-21 Sumitomo Electric Ind Ltd Carbon fiber reinforced composite material having coating
CN1102632A (en) * 1993-06-25 1995-05-17 株式会社日立制作所 Fibre reinforcement composite, making of same and unit made of same
CN104475741A (en) * 2014-12-17 2015-04-01 扬州大学 Method for preparing Ti5Si3 intermetallic compound powder by mechanical alloying

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH04119967A (en) * 1990-09-11 1992-04-21 Sumitomo Electric Ind Ltd Carbon fiber reinforced composite material having coating
CN1102632A (en) * 1993-06-25 1995-05-17 株式会社日立制作所 Fibre reinforcement composite, making of same and unit made of same
CN104475741A (en) * 2014-12-17 2015-04-01 扬州大学 Method for preparing Ti5Si3 intermetallic compound powder by mechanical alloying

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李明: "原位合成Ti5Si3基复合材料及其性能研究", 《中国优秀硕士学位论文全文数据库工程科技Ⅰ辑》 *
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114560713A (en) * 2022-03-01 2022-05-31 北京科技大学 Preparation method of carbon fiber toughened Ti-Si-C intermetallic compound composite material

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