CN105174899B - A kind of phosphate matrix composite and preparation method thereof - Google Patents
A kind of phosphate matrix composite and preparation method thereof Download PDFInfo
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- CN105174899B CN105174899B CN201510560535.9A CN201510560535A CN105174899B CN 105174899 B CN105174899 B CN 105174899B CN 201510560535 A CN201510560535 A CN 201510560535A CN 105174899 B CN105174899 B CN 105174899B
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Abstract
The invention discloses a kind of phosphate matrix composite and preparation method thereof, its preparation method comprises the following steps：Phosphate binders and kaolin are mixed and mechanical agitation, slurry is obtained；Prepare curing agent；By in the slurry obtained by curing agent addition step；Add high temperature resistant filler；Add wear resistant filler；Short quartz fibre is added in slurry, is uniformly mixed；By slurry at 100~120 DEG C 0.5~4h of precuring；Slurry after precuring is completed and cooled down is stirred, and obtains the pasty dough thing that flexibility is good, plasticity is strong；With 60~120MPa, 4~8h of hot pressing at 110~250 DEG C, phosphate matrix composite is obtained.The method flow of the present invention is short, and cost is low, and obtained composite material strength is high, and good toughness, high temperature resistant is resistant to chemical etching, wear-resisting.
Description
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 quartz fibre
Strengthen phosphate matrix composite and preparation method thereof.
Background technology
Composite be by the different material of two or more properties by physics and chemically composited, composition with two or
The material of two or more Phase stracture.Not only performance is better than any one single material in composition to the material, but also can
The special performance not having individually with component.Composite applies to aerospace field, auto industry, chemical industry, weaving and
Mechanical manufacturing field, medical science, sports equipment, building material field etc..
Composite can be divided into particulate reinforced composite and fibre reinforced composites according to reinforcing material.And particle increases
Strong composite is to increasing the DeGrain of toughness.
Composite can be divided into metal-base composites according to matrix classification, and ceramic matric composite, polymer matrix is combined
Material.Ceramic matric composite has intensity hardness high compared to metal-base composites, high temperature resistant, while having preferable chemistry
Stability.
Therefore ceramic base fiber reinforced composite material, with good application and popularization value.
Existing phosphate matrix material is generally bonded several forms by hydration and hardening, soda acid hardening and mineral, is also one
Kind of conventional binding agent, can be formed with the mixed preparing such as powder body material, fiber-like material and water.Phosphate is multiple with higher strong
Degree, low thermal coefficient of expansion, preferable inoxidizability, cure shrinkage is small, the advantage of room temperature curable.Quartz fibre has
Preferable heat endurance.Therefore quartz fibre enhancing phosphate matrix composite has higher real value.
The patent or the patent of mandate being disclosed, or the composite of correlation is reported in document.
The such as patent of invention of Application No. 201010550363.4, nano kaoline is modified twice, with polyethers
Glycol or polyester-diol are mixed and heated and ultrasonic disperse, obtain nano kaoline-PTMEG or polyester-diol compound,
For particle reinforced resin based composites.
The patent of invention of Application No. 200810050491.5, by PET, nucleator, vinyl is multifunctional and processing aid
After being mixed in twin-screw extrusion machine, basalt fibre is added, and after cobalt source is irradiated, composite is made, is fine
Tie up reinforced resin based composites.
The patent of invention of Application No. 03142206.3 is continuous lod by glass microballoon and nucleater modified mistake
Thermoplastic resin.
There is document report, phenolic resin and phosphate are mixed, add curing agent and base is made, impregnate alkali-free glass fiber cloth
Afterwards, prepreg is dried to obtain, prepreg is put into hot-forming in press, (the first and second authors, Zhang Degang, Zhou Yan, phenolic resin
The research of hydridization phosphate matrix composite, aerospace material technique, the 2nd phase in 2006).
There is document report, aluminium borate whisker strengthens the preparation of aluminophosphate-based electromagnetic wave transparent material, choose Aluminum phosphate powders and be used as base
Body, aluminium borate whisker prepares aluminium borate whisker/aluminium phosphate composite as reinforcement using normal pressure-sintered technique, (the first He
Second author, Lv Zhenyu, Geng Haoran, the preparation of the aluminophosphate-based electromagnetic wave transparent material of aluminium borate whisker enhancing, Science Bulletin, 2008,
Volume 53, the 13rd phase).
There is document report, use aluminium dihydrogen phosphate for matrix, aluminum oxide, aluminum phosphate is filler, prepare SiC reinforcement and answer
Condensation material, (the first and second authors, Wang Xinpeng, field is transplanted, and silicon carbide fibre strengthens preparation and the performance of aluminophosphate-based composite
Research, functional material, volume 11, the 36th phase in 2005).
The patent of invention of Application No. 201110110736.0, although phosphate and nano kaoline are raw materials, but use
Fiber be glass fibre, and kaolin is only modifying agent, and content is seldom.
The patent of invention of Application No. 201410481842.3 describes a kind of phosphate solution, metakaolin, adjustable solidification agent
And defoamer mixing, the mixture stirred, with carbon fiber, glass fibre and basalt fibre, one kind of aramid fiber
Or the composite and preparation method of assorted fibre.Metakaolin is that kaolin is calcined into 2 under 600~900 DEG C of temperature conditionss
Obtained after~20 hours, cost of material is big with respect to kaolin original soil；It is heating and curing using microwave and easily heats uneven, component chi
It is very little to be limited by microwave oven cavity size.Fiber is spread in layer, it is easy to cause anisotropy, and this patent is carried
The preparation method of confession is not only simple but also isotropism.Further, since the fiber added in this patent is quartz fibre, high temperature resistant
Property preferably, so material is overall also to have certain mechanical strength at high temperature.
The patent of invention of Application No. 201210312375.2 and Application No. 201210453554.8, phosphate matrix is not
Filling powder, and aluminium dihydrogen phosphate is easy to moisture absorption, dimensional stability is poor, there is big influence to room temperature strength.
The interface bond strength of fiber and matrix can neither too by force can not be too weak, have a document report, author is solidifying with colloidal sol
Glue method, prepares SiO2And Al2O3Colloidal sol, and quartz fiber surface is coated on, the fiber of film causes its turn through Overheating Treatment
Turn to SiO2And Al2O3Coating.Composite is prepared by prepreg moulding process, (the first and second authors, Zhou Yan, Guo Weihong,
The fiber film of phosphate matrix composite and the research of performance, functional material, supplementary issue (35) volume in 2004).The present invention is disclosed
Composite and preparation method thereof, the moderate strength that fiber is combined with basal body interface, which becomes, reveals obviously toughness.And
Composite disclosed by the invention and preparation method thereof, chemical resistance is good, and heat-resisting quantity is good, wear-resisting.
The content of the invention
For above-mentioned the deficiencies in the prior art, it is an object of the invention to provide a kind of phosphate matrix composite and its preparation
Method, toughness bad the problem of poor with the heat-resisting quantity for solving existing phosphate matrix composite presence.
To achieve the above object, the present invention uses following technical scheme：
A kind of preparation method of phosphate matrix composite, comprises the following steps：
(1) phosphate binders and kaolin are mixed and mechanical agitation, obtains slurry；
(2) curing agent is prepared；
(3) by the slurry obtained by curing agent addition step (1)；
(4) high temperature resistant filler is added in the slurry that step (3) is obtained；
(5) wear resistant filler is added in the slurry that step (4) is obtained；
(6) short quartz fibre is added in the slurry that step (5) is obtained, be uniformly mixed；
(7) slurry for obtaining step (6) 0.5~4h of precuring at 100~120 DEG C,
(8) slurry after precuring being completed and cooled down is stirred, and obtains the pasty state that flexibility is good, plasticity is strong
Dough thing；
(9) 4~8h of hot pressing at 110~250 DEG C, obtains phosphate matrix composite.
Further, in the step (1), phosphate binders are that aluminium dihydrogen phosphate aqueous solution, the hydrogen aluminium of phosphoric acid one are water-soluble
A kind of or their mixture in liquid.
Further, in the step (1), kaolin is soft kaolin or hard kaolin, or both mixtures.
Further, in the step (1), solute and kaolinic mass ratio are 2 in aqueous phosphatic:1~1:1.
Further, in the step (2), curing agent is by a kind of either two kinds of powder of powder in magnesia, zinc oxide
End mixture and according to mass ratio be mixture of powders：Water=1：2~1：5 ratio planetary ball mill ball milling 20min
~60min is made.
Further, in the step (3), the addition of curing agent be Solute mass in aqueous phosphatic 10~
40%.
Further, in the step (3), it is 0.2~1.0g/min that curing agent, which adds phosphatic speed, to prevent production
Raw uneven floccule.
Further, in the step (4), high temperature resistant filler be one kind in aluminum oxide, silica, zirconium oxide or
It is the mixture of several powder.
Further, in the step (4), the addition of high temperature resistant filler for aqueous phosphatic quality 10~
30%.
Further, in the step (5), during wear resistant filler is carborundum, titanium carbide, tungsten carbide, niobium carbide, ramet
A kind of or several powder mixture.
Further, in the step (5), the addition of wear resistant filler for aqueous phosphatic Solute mass 10~
30%.
Further, in the step (6), the addition of quartz fibre is solute and kaolinic in aqueous phosphatic
The 10~25% of gross mass.
Further, in step (7), in procuring process, apply stirring or shaken well treatment measures to prevent slurry
Material is local to be hardened.
A kind of phosphate matrix composite being made up of above-mentioned method.
The beneficial effects of the invention are as follows：
The present invention is using the method for short fiber reinforced phosphate base, obtained composite isotropism；Again because of phosphoric acid
Salt, kaolin, and quartz fibre resistance to elevated temperatures in itself and anti-phosphate chemical corrosivity are excellent, so composite is in itself
Still there is certain mechanical strength at high temperature, and it is resistant to chemical etching, and again because adding wear resistant filler and kaolin, this hair
Composite-material abrasive prepared by bright disclosed material preparation method, water-tolerant.Slurry after precuring is completed and cooled down enters
Row stir process, obtains flexibility is good, plasticity is strong pasty dough thing, and the step causes in the feed can be without disappearing
Infusion and dispersant.
The preparation method of this patent has flow short, and the low advantage of energy consumption, obtained composite chemical resistance is good,
Heat-resisting quantity is good, wear-resisting.
Brief description of the drawings
Fig. 1 is maximum stress-displacement curve in embodiment 2 at room temperature；
Fig. 2 is maximum stress-displacement curve in embodiment 4 at room temperature；
Fig. 3 is 300 DEG C of experience, 2 10min maximum stress-displacement curve in embodiment 4；
Fig. 4 is 500 DEG C of experience, 1 10min maximum stress-displacement curve in embodiment 4；
Fig. 5 is 700 DEG C of experience, 1 10min maximum stress-displacement curve in embodiment 4.
Embodiment
The present invention is further described with reference to specific embodiment.
Embodiment 1
According to mass fraction, 10 parts of hydrogen aluminum water solutions of phosphoric acid one and 5 parts of soft kaolin stir, and obtain slurry, wherein
Solutes content is 50% in the hydrogen aluminum water solution of phosphoric acid one；0.3 part of magnesia is taken, 0.7 part of water is prepared in ball mill ball milling 40min
Curing agent；Curing agent is added in slurry with 0.5g/min speed, and stirred；1 part of aluminum oxide of addition, 1 part of carborundum,
Stir；The precuring 1h at 120 DEG C, applies the Homogenization Treatments measure such as stirring or vibration to prevent slurry local if necessary
It is hardened；With 90MPa hot pressing 4h at 120 DEG C；Its intensity at room temperature is measured, and passes through 300 DEG C, 500 DEG C, 700 DEG C of difference 1
Secondary 10min, 2 10min, the intensity after 3 10min calcinations, room temperature strength is 49MPa, and remainder data is shown 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 hydrogen aluminum water solutions of phosphoric acid one and 10 parts of hard kaolinites
Soil stirs, and wherein solutes content is 30% in aqueous phosphatic；Take 0.75 part of zinc oxide, 2.25 parts of water, in ball milling
Machine ball milling 50min prepares curing agent；Curing agent is added in slurry with 0.4g/min speed, and stirred；Add oxidation
2 parts of aluminium, 2 parts of niobium carbide, stirs；The precuring 1.5h at 120 DEG C, applies the Homogenization Treatments such as stirring or vibration if necessary
Measure is to prevent slurry to be locally hardened；With 60MPa hot pressing 7h at 120 DEG C；Its intensity at room temperature is measured, and passes 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, its
Remainder evidence is shown 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, 30mm quartz fibres are added in embodiment 3, curing agent is 0.2 part of magnesia, 0.8 part of water,
Curing agent is prepared in ball mill ball milling 20min, curing agent is added in slurry with 0.8g/min speed..2 parts of silica 1,
1.4 parts of tungsten carbide.The precuring 40min at 120 DEG C, with 120MPa hot pressing 5h at 120 DEG C.Remaining raw material proportioning and intensity
3 and table 4 are shown in Table, solutes content is 60% wherein in aqueous phosphatic, and all components are 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 hydrogen aluminum water solutions of phosphoric acid one and 10 parts of soft kaolinites
Soil stirs, and wherein solutes content is 50% in aqueous phosphatic；Take 0.5 part of zinc oxide, 0.5 part of magnesia, water 5
Part, prepare curing agent in ball mill ball milling 30min；Curing agent is added in slurry with 0.8g/min speed, and stirred；
4 parts of zirconium oxide is added, 5 parts of niobium carbide stirs；Plus 6 parts of 30mm quartz fibres；The precuring 2h at 120 DEG C, 120
DEG C with 70MPa hot pressing 5h；Room temperature strength is 35MPa, and remaining rupture strength value is shown 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 maximum stress-displacement curve figure of embodiment, and wherein maximum stress can be expressed from the next
Wherein F is loading force, and L is span between lower fulcrum, and b is specimen width, and h is sample thickness.
It can be seen that the sample come in Fig. 1 does not have fiber, so not showing toughness, and in Fig. 2~Fig. 4, stone is added
After English fiber, minimum, sample fracture are being reduced to without being horse back after maximum stress reaches maximum, but have a gradient slow
Ground declines, and this is the performance of flexible.Even maximum stress after maximum is reached, goes out again during reduction in figs. 2 and 3
Increased phenomenon is showed, the reason for this is substantially because of spike protein gene.
Comparative example
According to mass fraction, 8 parts of aluminium dihydrogen phosphate aqueous solution, wherein 2 parts of one hydrogen aluminum water solution of phosphoric acid, aqueous phosphatic
Solutes content be 30%, aluminium hydroxide, phosphoric acid, nitric acid, ammonium dihydrogen phosphate, carborundum, cupric oxide, iron oxide each takes respectively
1 part, 2 parts, 3 parts, 4 parts, 5 parts, 6 parts, 7 parts, and respectively at 100 DEG C, 200 DEG C, 300 DEG C, 24h is passed through in heating 8h solidifications, discovery
Whole moisture absorptions are serious afterwards, and shape can not be kept.But the equal water-tolerant of 1~embodiment of embodiment 4, shape remains intact.
Described above is only some embodiments of the present invention, it should be pointed out that：For the ordinary skill people of the art
For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (1)
1. a kind of preparation method of phosphate matrix composite, it is characterised in that：Comprise the following steps：
（1）Phosphate binders and kaolin are mixed and mechanical agitation, slurry is obtained；Phosphate binders are aluminium dihydrogen phosphates
A kind of or their mixture in the aqueous solution, the hydrogen aluminum water solution of phosphoric acid one；Kaolin is soft kaolin or hard kaolin, or
Person is both mixtures；Solute and kaolinic mass ratio in aqueous phosphatic are 2:1~1:1；
（2）Prepare curing agent；Curing agent for powder is mixed by magnesia, the mixture of two kinds of powder of zinc oxide and according to mass ratio
Thing：Water=1：2~1：5 ratio is made with planetary ball mill ball milling 20min~60min；
（3）Curing agent is added into step（1）In resulting slurry；The addition of curing agent is solute matter in aqueous phosphatic
The 10~40% of amount；It is 0.2~1.0g/min that curing agent, which adds phosphatic speed,；
（4）In step（3）High temperature resistant filler is added in obtained slurry；High temperature resistant filler is aluminum oxide, silica, zirconium oxide
In a kind of or several powder mixture；The addition of high temperature resistant filler is 10 of Solute mass in aqueous phosphatic
~30%；
（5）In step（4）Wear resistant filler is added in obtained slurry；Wear resistant filler is carborundum, titanium carbide, tungsten carbide, carbonization
The mixture of a kind of or several powder in niobium, ramet；The addition of wear resistant filler is solute in aqueous phosphatic
The 10~30% of quality；
（6）Short quartz fibre is added into step（5）In obtained slurry, it is uniformly mixed；The addition of quartz fibre is phosphorus
The 10~25% of solute and kaolinic gross mass in acid salt aqueous solution；
（7）By step（6）Obtained slurry 0.5~4h of precuring at 100~120 DEG C；In procuring process, apply stirring or
Shaken well treatment measures；
（8）Slurry after precuring is completed and cooled down is stirred, and obtains the pasty dough that flexibility is good, plasticity is strong
Thing；
（9）With pressure 60~120MPa, 4~8h of hot pressing at 110~250 DEG C, phosphate matrix composite is obtained.
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| 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 |
| CN111807808B (en) * | 2020-08-11 | 2022-04-22 | 哈尔滨工业大学 | Preparation method of high-temperature-resistant heat-insulation composite material |
| CN113321483B (en) * | 2021-06-03 | 2023-02-03 | 哈尔滨工程大学 | Preparation method of heating-free broken quartz fiber cloth reinforced phosphate composite material |
| CN113800863B (en) * | 2021-08-26 | 2022-12-16 | 北京工业大学 | Modified recycled aggregate concrete with electromagnetic wave-transmitting function and preparation method thereof |
| CN114394775A (en) * | 2022-01-20 | 2022-04-26 | 南华大学 | Kaolin-based curing agent and preparation method and application thereof |
| CN116462502A (en) * | 2022-10-04 | 2023-07-21 | 汶川县神州锆业科技有限公司 | High-temperature-resistant and electric corrosion-resistant method for special equipment |
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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 |
| CN102010671B (en) * | 2010-09-13 | 2013-12-11 | 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 |
| CN102503499B (en) * | 2011-10-17 | 2013-06-12 | 中国烟草中南农业试验站 | Inorganic non-metal compound material for heating system and preparation method thereof |
| CN102514346B (en) * | 2011-12-19 | 2014-08-13 | 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 |
| CN104228184B (en) * | 2014-09-19 | 2015-12-02 | 深圳大学 | A kind of phosphate base fibrous composite and preparation method thereof |
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