CN105174899A - Phosphate-based composite material and preparation method thereof - Google Patents

Phosphate-based composite material and preparation method thereof Download PDF

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CN105174899A
CN105174899A CN201510560535.9A CN201510560535A CN105174899A CN 105174899 A CN105174899 A CN 105174899A CN 201510560535 A CN201510560535 A CN 201510560535A CN 105174899 A CN105174899 A CN 105174899A
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phosphate
slurry
matrix composite
phosphate matrix
resistant filler
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CN105174899B (en
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刘玉付
沈杰
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Southeast University
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Southeast University
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Abstract

The invention discloses a phosphate-based composite material and a preparation method thereof. The preparation method of the composite material comprises the following steps: mixing a phosphate adhesive with kaolin, and mechanically stirring to obtain a slurry; preparing a curing agent; adding the curing agent to the obtained slurry; adding a high temperature resistant filler; adding a wear resistant filler; adding short quartz fibers to the obtained slurry, and stirring until uniform mixing; pre-curing the obtained slurry at 100-120DEG C for 0.5-4h; cooling, stirring the pre-cured and cooled slurry to obtain a pasty dough-shaped material with good flexibility and strong plasticity; and carrying out hot pressing at 110-250DEG C under 60-120MPa for 4-8h to obtain the phosphate-based composite material. The method has the advantages of short flow and low cost, and the composite material prepared in the invention has the advantages of high strength, good toughness, high temperature resistance, chemical corrosion resistance and wear resistance.

Description

A kind of phosphate matrix composite and preparation method thereof
Technical field
The present invention relates to a kind of phosphate matrix composite and preparation method thereof, particularly a kind of resistant to elevated temperatures silica fiber strengthens phosphate matrix composite and preparation method thereof.
Background technology
Matrix material is by the material of two or more different in kinds by physics and chemistry compound, and composition has the material of two or more Phase stracture.This material not only performance be better than forming in any one independent material, but also the special performance that component do not have separately can be had.Matrix material applies to aerospace field, automotive industry, chemical industry, weaving and mechanical manufacturing field, medical science, sports equipment, building material field etc.
Matrix material can be divided into particulate reinforced composite and fibre reinforced composites according to strongthener.And particulate reinforced composite is to the DeGrain increasing toughness.
Matrix material can be divided into metal-base composites, ceramic matric composite, polymer matrix composite according to matrix classification.Metal-base composites compared by ceramic matric composite, and to have intensity hardness high, high temperature resistant, has good chemical stability simultaneously.
Therefore ceramic base fibre reinforced composites, have good application and popularization value.
Existing phosphate matrix material is hardened and several form of mineral bonding by hydration and hardening, soda acid usually, is also a kind of conventional binding agent, can form with the mixed preparing such as powder body material, fiber-like material and water.Phosphoric acid salt has higher intensity again, low thermal expansivity, good oxidation-resistance, and cure shrinkage is little, the advantage of curable at ambient temperature.Silica fiber has good thermostability.Therefore silica fiber enhancing phosphate matrix composite has higher actual value.
The patent of existing disclosed patent or mandate, or in document, report relevant matrix material.
Such as application number is the patent of invention of 201010550363.4, nano kaoline is carried out twice modification, mixing with polyether glycol or polyester glycol and heat and ultrasonic disperse, obtaining nano kaoline-polyether glycol or polyester glycol mixture, is particle reinforce polymer matrix composites.
Application number is the patent of invention of 200810050491.5, by PET, and nucleator, after the multifunctional and processing aid of vinyl mixes in twin-screw extrusion machine, then add basalt fibre, and after cobalt-60 radiosterilize, obtained matrix material is fiber-reinforced resin matrix compound material.
Application number is the patent of invention of 03142206.3, is continuous lod by the thermoplastic resin of glass microballon and nucleater modified mistake.
There is bibliographical information, by resol and phosphoric acid salt mixing, add solidifying agent and obtain base, after dipping alkali-free glass fiber cloth, dry to obtain prepreg, it is hot-forming that prepreg puts into press, (the first and second authors, Zhang Degang, Zhou Yan, the research of resol hydridization phosphate matrix composite, aerospace material technique, the 2nd phase in 2006).
Have bibliographical information, aluminium borate whisker strengthens the preparation of aluminophosphate-based electromagnetic wave transparent material, chooses Aluminum phosphate powders as matrix, aluminium borate whisker is as reinforcement, normal pressure-sintered technique is adopted to prepare aluminium borate whisker/aluminium phosphate composite, (the first and second authors, Lv Zhenyu, Geng Haoran, aluminium borate whisker strengthens the preparation of aluminophosphate-based electromagnetic wave transparent material, Science Bulletin, 2008,53rd volume, the 13rd phase).
Have bibliographical information, employing aluminium dihydrogen phosphate is matrix, aluminum oxide, aluminum phosphate is filler, prepare SiC reinforcement matrix material, (the first and second authors, Wang Xinpeng, field is transplanted, silicon carbide fiber strengthens preparation and the performance study of aluminophosphate-based matrix material, functional materials, 2005,11st volume, the 36th phase).
Application number is the patent of invention of 201110110736.0, although phosphoric acid salt and nano kaoline are raw materials, fiber be glass fibre, and kaolin is only properties-correcting agent, and content is little.
Application number be 201410481842.3 patent of invention describe the mixing of a kind of phosphate solution, metakaolin, adjustable solidification agent and defoamer, the mixture that stirs, with carbon fiber, glass fibre and basalt fibre, the matrix material of a kind of or assorted fibre of aramid fiber and preparation method.Metakaolin is calcined by kaolin after 2 ~ 20 hours to obtain under 600 ~ 900 DEG C of temperature condition, and raw materials cost is large relative to kaolin original soil; Easily heating is uneven, scantling is subject to microwave oven cavity limitation of size to use microwave heating to solidify.Fiber is in layer spread, and is easy to cause anisotropy, and the preparation method provided of this patent not only simple but also isotropy.In addition, because the fiber added in this patent is silica fiber, high thermal resistance is better, so material monolithic at high temperature also has certain mechanical strength.
Application number be 201210312375.2 and application number be the patent of invention of 201210453554.8, the non-filling powder of phosphate matrix, and aluminium dihydrogen phosphate is easy to moisture absorption, dimensional stability is poor, has large impact to room temperature strength.
The interface bond strength of fiber and matrix can not too by force can not be too weak, has bibliographical information, author with sol-gel method, preparation SiO 2and Al 2o 3colloidal sol, and be coated on quartz fiber surface, the fiber of film makes it be converted into SiO through Overheating Treatment 2and Al 2o 3coating.Matrix material is prepared, (the first and second authors, Zhou Yan, Guo Weihong, the fiber film of phosphate matrix composite and the research of performance, functional materials, supplementary issue (35) volume in 2004) by prepreg moulding process.Matrix material disclosed by the invention and preparation method thereof, the moderate strength that fiber is combined with basal body interface cashes out obviously toughness.And matrix material disclosed by the invention and preparation method thereof, chemical resistance is good, and high thermal resistance is good, wear-resisting.
Summary of the invention
For above-mentioned the deficiencies in the prior art, the object of this invention is to provide a kind of phosphate matrix composite and preparation method thereof, poor with the high thermal resistance solving the existence of existing phosphate matrix composite, the problem that toughness is bad.
For achieving the above object, the present invention is by the following technical solutions:
A preparation method for phosphate matrix composite, comprises the following steps:
(1) by phosphate binders and kaolin mixing also mechanical stirring, slurry is obtained;
(2) solidifying agent is prepared;
(3) solidifying agent is added in the slurry that step (1) obtains;
(4) high temperature resistant filler is added in the slurry obtained in step (3);
(5) wear resistant filler is added in the slurry obtained in step (4);
(6) short silica fiber is added in the slurry that step (5) obtains, be uniformly mixed;
(7) the slurry Procuring 0.5 ~ 4h at 100 ~ 120 DEG C step (6) obtained,
(8) Procuring to be completed and cooled slurry carries out stir process, obtain the pasty dough thing that flexibility is good, plasticity-is strong;
(9) hot pressing 4 ~ 8h at 110 ~ 250 DEG C, obtains phosphate matrix composite.
Further, in described step (1), phosphate binders is a kind of in aluminium dihydrogen phosphate aqueous solution, phosphoric acid one hydrogen aluminum water solution or their mixture.
Further, in described step (1), kaolin is soft kaolin or hard kaolin, or both mixtures.
Further, in described step (1), in aqueous phosphatic, solute and kaolinic mass ratio are 2:1 ~ 1:1.
Further, in described step (2), solidifying agent by a kind of powder in magnesium oxide, zinc oxide or two kinds of powder mixture and be powdered mixture according to mass ratio: the ratio planetary ball mill ball milling 20min ~ 60min of water=1:2 ~ 1:5 obtains.
Further, in described step (3), the add-on of solidifying agent is 10 ~ 40% of Solute mass in aqueous phosphatic.
Further, in described step (3), it is 0.2 ~ 1.0g/min that solidifying agent adds phosphatic speed, to prevent uneven floss.
Further, in described step (4), high temperature resistant filler is the mixture of a kind of or several powder in aluminum oxide, silicon-dioxide, zirconium white.
Further, in described step (4), the add-on of high temperature resistant filler is 10 ~ 30% of aqueous phosphatic quality.
Further, in described step (5), wear resistant filler is the mixture of a kind of or several powder in silicon carbide, titanium carbide, wolfram varbide, niobium carbide, tantalum carbide.
Further, in described step (5), the add-on of wear resistant filler is 10 ~ 30% of aqueous phosphatic Solute mass.
Further, in described step (6), the add-on of silica fiber is 10 ~ 25% of solute and kaolinic total mass in aqueous phosphatic.
Further, in step (7), in Procuring process, applying stirring or shaken well treatment measures are in case grouting material local is hardening.
A kind of phosphate matrix composite be made up of above-mentioned method.
The invention has the beneficial effects as follows:
The present invention adopts the method for short fiber reinforced phosphate base, the matrix material isotropy obtained; Again because, phosphoric acid salt, kaolin, with the resistance to elevated temperatures of silica fiber itself and anti-phosphate chemical corrodibility excellent, so matrix material itself at high temperature still has certain mechanical strength, and resistance to chemical attack, and again because add wear resistant filler and kaolin, composite-material abrasive prepared by material preparation method disclosed by the invention, water-tolerant.Complete Procuring and cooled slurry carries out stir process, obtain the pasty dough thing that flexibility is good, plasticity-is strong, this step makes can not add defoamer and dispersion agent in the feed.
It is short that the preparation method of this patent has flow process, and the advantage that energy consumption is low, obtained matrix material chemical resistance is good, and high thermal resistance is good, wear-resisting.
Accompanying drawing explanation
Fig. 1 is the maximum stress-displacement curve in embodiment 2 under room temperature;
Fig. 2 is the maximum stress-displacement curve in embodiment 4 under room temperature;
Fig. 3 experiences 300 DEG C, the maximum stress-displacement curve of 2 10min in embodiment 4;
Fig. 4 experiences 500 DEG C, the maximum stress-displacement curve of 1 10min in embodiment 4;
Fig. 5 experiences 700 DEG C, the maximum stress-displacement curve of 1 10min in embodiment 4.
Embodiment
Below in conjunction with specific embodiment, the present invention is further described.
Embodiment 1
According to mass fraction, 10 parts of phosphoric acid one hydrogen aluminum water solutions and 5 parts of soft kaolin stir, and obtain slurry, and wherein in phosphoric acid one hydrogen aluminum water solution, solutes content is 50%; Get 0.3 part, magnesium oxide, 0.7 part, water, prepare solidifying agent at ball mill ball milling 40min; Solidifying agent is added in slurry with the speed of 0.5g/min, and stirs; Add 1 part, aluminum oxide, 1 part, silicon carbide, stirs; Procuring 1h at 120 DEG C, applies the Homogenization Treatments measures such as stirring or vibration if desired in case grouting material local is hardening; With 90MPa hot pressing 4h at 120 DEG C; Measure its intensity at room temperature, and through 300 DEG C, 500 DEG C, 700 DEG C of difference, 1 10min, 2 10min, the intensity after 3 10min calcinations, room temperature strength is 49MPa, and remainder data is in table 1.
Table 1
Intensity/MPa 300℃ 500℃ 700℃
1 10min 18 11 7
2 10min 29 20 6
3 10min 42 15 2
Embodiment 2
According to mass fraction, by 30 parts of aluminium dihydrogen phosphate aqueous solutions, 20 parts of phosphoric acid one hydrogen aluminum water solutions and 10 parts of hard kaolin stir, and wherein in aqueous phosphatic, solutes content is 30%; Get 0.75 part, zinc oxide, 2.25 parts, water, prepare solidifying agent at ball mill ball milling 50min; Solidifying agent is added in slurry with the speed of 0.4g/min, and stirs; Add 2 parts, aluminum oxide, niobium carbide 2 parts, stirs; Procuring 1.5h at 120 DEG C, applies the Homogenization Treatments measures such as stirring or vibration if desired in case grouting material local is hardening; With 60MPa hot pressing 7h at 120 DEG C; Measure its intensity at room temperature, and through 300 DEG C, 500 DEG C, 700 DEG C of difference, 1 10min, 2 10min, the intensity after 3 10min calcinations, room temperature strength is 43MPa, and remainder data is in table 2.
Table 2
Intensity/MPa 300℃ 500℃ 700℃
1 10min 18 18 9
2 10min 13 4 4
3 10min 22 14 6
Embodiment 3
According to mass fraction, add 30mm silica fiber in embodiment 3, solidifying agent is 0.2 part, magnesium oxide, and 0.8 part, water is prepared solidifying agent at ball mill ball milling 20min, added in slurry by solidifying agent with the speed of 0.8g/min.Silica 1 .2 part, wolfram varbide 1.4 parts.Procuring 40min at 120 DEG C, with 120MPa hot pressing 5h at 120 DEG C.Remaining proportioning raw materials and intensity are in table 3 and table 4, and wherein in aqueous phosphatic, solutes content is 60%, and all components is all according to mass fraction meter.
Table 3
Table 4
Embodiment 4
According to mass fraction, by 12 parts of aluminium dihydrogen phosphate aqueous solutions, 28 parts of phosphoric acid one hydrogen aluminum water solutions and 10 parts of soft kaolin stir, and wherein in aqueous phosphatic, solutes content is 50%; Get 0.5 part, zinc oxide, 0.5 part, magnesium oxide, 5 parts, water, prepare solidifying agent at ball mill ball milling 30min; Solidifying agent is added in slurry with the speed of 0.8g/min, and stirs; Add zirconium white 4 parts, niobium carbide 5 parts, stirs; Add 6 parts of 30mm silica fibers; Procuring 2h at 120 DEG C, at 120 DEG C with 70MPa hot pressing 5h; Room temperature strength is 35MPa, and remaining folding strength value is in table 5.
Table 5
Intensity/MPa 300℃ 500℃ 700℃
1 10min 21 1 7
2 10min 26 6 6
3 10min 13 7 4
Fig. 1 ~ Fig. 5 is the maximum stress-displacement curve figure of embodiment, and wherein maximum stress can be expressed from the next
σ = 3 F L 2 bh 2
Wherein F is loading force, and L is span between lower fulcrum, and b is specimen width, and h is sample thickness.
The sample can found out in Fig. 1 does not have fiber, so do not show toughness, and in Fig. 2 ~ Fig. 4, after having added silica fiber, maximum stress reach maximum after be not be just reduced at once minimum, sample fracture, but having a gradient to decline lentamente, this is the performance of flexible.Even in figs. 2 and 3 maximum stress reach maximum after, in reduction process, to have occurred again the phenomenon increased, this is obviously because the reason of spike protein gene.
Comparative example
According to mass fraction, aluminium dihydrogen phosphate aqueous solution 8 parts, phosphoric acid one hydrogen aluminum water solution 2 parts, wherein the solutes content of aqueous phosphatic is 30%, aluminium hydroxide, phosphoric acid, nitric acid, primary ammonium phosphate, silicon carbide, cupric oxide, ferric oxide gets 1 part separately respectively, 2 parts, 3 parts, 4 parts, 5 parts, 6 parts, 7 parts, again respectively at 100 DEG C, 200 DEG C, 300 DEG C, heating 8h solidification, find that whole moisture absorption is serious after 24h, shape can not keep.But embodiment 1 ~ embodiment 4 is water-tolerant all, and form trait is intact.
The above is only some embodiments of the present invention; be noted that for those skilled in the art; under the premise without departing from the principles of the invention, can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.

Claims (10)

1. a preparation method for phosphate matrix composite, is characterized in that: comprise the following steps:
(1) by phosphate binders and kaolin mixing also mechanical stirring, slurry is obtained;
(2) solidifying agent is prepared;
(3) solidifying agent is added in the slurry that step (1) obtains;
(4) high temperature resistant filler is added in the slurry obtained in step (3);
(5) wear resistant filler is added in the slurry obtained in step (4);
(6) short silica fiber is added in the slurry that step (5) obtains, be uniformly mixed;
(7) the slurry Procuring 0.5 ~ 4h at 100 ~ 120 DEG C step (6) obtained,
(8) Procuring to be completed and cooled slurry carries out stir process, obtain the pasty dough thing that flexibility is good, plasticity-is strong;
(9) at 110 ~ 250 DEG C with pressure 60 ~ 120MPa hot pressing 4 ~ 8h, obtain phosphate matrix composite.
2. the preparation method of phosphate matrix composite as claimed in claim 1, is characterized in that: in described step (1), and phosphate binders is a kind of in aluminium dihydrogen phosphate aqueous solution, phosphoric acid one hydrogen aluminum water solution or their mixture; Kaolin is soft kaolin or hard kaolin, or both mixtures.
3. the preparation method of phosphate matrix composite as claimed in claim 1, it is characterized in that: in described step (1), the solute in aqueous phosphatic and kaolinic mass ratio are 2:1 ~ 1:1.
4. the preparation method of phosphate matrix composite as claimed in claim 1, it is characterized in that: in described step (2), solidifying agent by a kind of powder in magnesium oxide, zinc oxide or two kinds of powder mixture and be powdered mixture according to mass ratio: the ratio planetary ball mill ball milling 20min ~ 60min of water=1:2 ~ 1:5 obtains.
5. the preparation method of phosphate matrix composite as claimed in claim 1, it is characterized in that: in described step (3), the add-on of solidifying agent is 10 ~ 40% of Solute mass in aqueous phosphatic; It is 0.2 ~ 1.0g/min that solidifying agent adds phosphatic speed.
6. the preparation method of phosphate matrix composite as claimed in claim 1, it is characterized in that: in described step (4), high temperature resistant filler is the mixture of a kind of or several powder in aluminum oxide, silicon-dioxide, zirconium white; The add-on of high temperature resistant filler is 10 ~ 30% of Solute mass in aqueous phosphatic.
7. the preparation method of phosphate matrix composite as claimed in claim 1, it is characterized in that: in described step (5), wear resistant filler is the mixture of a kind of or several powder in silicon carbide, titanium carbide, wolfram varbide, niobium carbide, tantalum carbide; The add-on of wear resistant filler is 10 ~ 30% of Solute mass in aqueous phosphatic.
8. the preparation method of phosphate matrix composite as claimed in claim 1, is characterized in that: in described step (6), and the add-on of silica fiber is 10 ~ 25% of solute and kaolinic total mass in aqueous phosphatic.
9. the preparation method of phosphate matrix composite as claimed in claim 1, is characterized in that: in step (7), in Procuring process, applies to stir or shaken well treatment measures.
10. the phosphate matrix composite be made up of the arbitrary described method of claim 1-9.
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106316263A (en) * 2016-08-24 2017-01-11 北京中交桥宇科技有限公司 Anti-abrasion concrete
CN108083665A (en) * 2018-01-31 2018-05-29 河南东大高温节能材料有限公司 A kind of aluminium dihydrogen phosphate-silicon powder combined high temperature binding agent and preparation method thereof

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CN1673169A (en) * 2005-03-15 2005-09-28 华南理工大学 Process of preparing mineral bonding material and its composite material with phosphate and aluminium-silicon material
CN102010671A (en) * 2010-09-13 2011-04-13 天津浦安防火科技有限公司 High-temperature resisting inorganic adhesive specially used for bonding pearlite fireproof plate with steel plate
CN102503499A (en) * 2011-10-17 2012-06-20 中国烟草中南农业试验站 Inorganic non-metal compound material for heating system and preparation method thereof
CN102514346A (en) * 2011-12-19 2012-06-27 西南科技大学 Preparation method of quartz fiber/chrome aluminum phosphate-based high temperature wave-transmitting material
CN102617059A (en) * 2012-03-23 2012-08-01 深圳大学 Phosphate base cementing agent
CN104228184A (en) * 2014-09-19 2014-12-24 深圳大学 Phosphate based fiber composite and preparation method thereof

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1673169A (en) * 2005-03-15 2005-09-28 华南理工大学 Process of preparing mineral bonding material and its composite material with phosphate and aluminium-silicon material
CN102010671A (en) * 2010-09-13 2011-04-13 天津浦安防火科技有限公司 High-temperature resisting inorganic adhesive specially used for bonding pearlite fireproof plate with steel plate
CN102503499A (en) * 2011-10-17 2012-06-20 中国烟草中南农业试验站 Inorganic non-metal compound material for heating system and preparation method thereof
CN102514346A (en) * 2011-12-19 2012-06-27 西南科技大学 Preparation method of quartz fiber/chrome aluminum phosphate-based high temperature wave-transmitting material
CN102617059A (en) * 2012-03-23 2012-08-01 深圳大学 Phosphate base cementing agent
CN104228184A (en) * 2014-09-19 2014-12-24 深圳大学 Phosphate based fiber composite and preparation method thereof

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106316263A (en) * 2016-08-24 2017-01-11 北京中交桥宇科技有限公司 Anti-abrasion concrete
CN106316263B (en) * 2016-08-24 2018-06-05 北京中交桥宇科技有限公司 A kind of abrasion-proof concrete
CN108083665A (en) * 2018-01-31 2018-05-29 河南东大高温节能材料有限公司 A kind of aluminium dihydrogen phosphate-silicon powder combined high temperature binding agent and preparation method thereof

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