CN113321483A - Preparation method of heating-free broken quartz fiber cloth reinforced phosphate composite material - Google Patents

Preparation method of heating-free broken quartz fiber cloth reinforced phosphate composite material Download PDF

Info

Publication number
CN113321483A
CN113321483A CN202110620473.1A CN202110620473A CN113321483A CN 113321483 A CN113321483 A CN 113321483A CN 202110620473 A CN202110620473 A CN 202110620473A CN 113321483 A CN113321483 A CN 113321483A
Authority
CN
China
Prior art keywords
fiber cloth
phosphate
quartz fiber
composite material
heating
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN202110620473.1A
Other languages
Chinese (zh)
Other versions
CN113321483B (en
Inventor
张春红
曹先启
刘立佳
张嘉明
彭程
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Harbin Engineering University
Original Assignee
Harbin Engineering University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Harbin Engineering University filed Critical Harbin Engineering University
Priority to CN202110620473.1A priority Critical patent/CN113321483B/en
Publication of CN113321483A publication Critical patent/CN113321483A/en
Application granted granted Critical
Publication of CN113321483B publication Critical patent/CN113321483B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B28/00Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
    • C04B28/34Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing cold phosphate binders
    • C04B28/344Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing cold phosphate binders the phosphate binder being present in the starting composition solely as one or more phosphates
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/00241Physical properties of the materials not provided for elsewhere in C04B2111/00
    • C04B2111/0037Materials containing oriented fillers or elements
    • C04B2111/00379Materials containing oriented fillers or elements the oriented elements being fibres
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/20Resistance against chemical, physical or biological attack
    • C04B2111/28Fire resistance, i.e. materials resistant to accidental fires or high temperatures

Abstract

The invention discloses a preparation method of a heating-free broken quartz fiber cloth reinforced phosphate composite material, and relates to the field of preparation methods of phosphate composite materials. The invention aims to solve the technical problems of corrosion of a vacuum bag, complex curing process and poor interlayer bonding force in the heating and curing process of the current two-dimensional quartz fiber cloth reinforced phosphate-based composite material. The method comprises the following steps: preparing a modified non-aqueous phosphate adhesive matrix; preparing a curing agent; mixing and stirring the two into a uniform paste to obtain the phosphate adhesive; and (3) soaking the quartz fiber cloth in the fiber treating agent, cutting the quartz fiber cloth into quartz fiber cloth blocks, mixing the quartz fiber cloth blocks with a phosphate adhesive, and curing at normal temperature. The invention adopts the phosphate adhesive cured at normal temperature, can solve the problems of volatilization of a phosphate solvent cured by heating to corrode a vacuum bag, difficult pressure maintaining and the like, and the prepared composite material heat-resistant quartz fiber cloth reinforced phosphate composite material has equivalent mechanical properties and simpler preparation process. The method is used for preparing the phosphate composite material.

Description

Preparation method of heating-free broken quartz fiber cloth reinforced phosphate composite material
Technical Field
The invention relates to the field of preparation methods of phosphate composite materials.
Background
The current aerospace technology is rapidly developed, the flying Mach number of an aircraft is continuously improved, the requirement for bearing heat-resistant composite materials is increasingly large, and therefore, the development of novel heat-resistant composite materials is of great significance. The phosphate cementing material has the characteristics of excellent high temperature resistance, designability of structure and the like, and is one of the preferred cementing materials for the heat-resistant composite material. The commonly used two-dimensional quartz fiber cloth reinforced phosphate-based composite material at present has the technical problems of corrosion of a vacuum bag in the heating and curing process, complex curing process and poor interlayer bonding force, and the application and development of the phosphate composite material are hindered.
Disclosure of Invention
The invention provides a preparation method of a heating-free broken quartz fiber cloth reinforced phosphate composite material, aiming at solving the technical problems of corrosion of a vacuum bag, complex curing process and poor interlayer bonding force in the heating and curing process of the current two-dimensional quartz fiber cloth reinforced phosphate composite material.
A preparation method of a heating-free broken quartz fiber cloth reinforced phosphate composite material comprises the following steps:
heating an industrial grade chromium dihydrogen phosphate aluminum solution to obtain a saturated salt solution, controlling the heating temperature to be 78-82 ℃, then cooling to-18-20 ℃, keeping for 12-13 h, crystallizing chromium dihydrogen phosphate aluminum at the bottom, freezing the upper layer, and separating ice to obtain crystallized chromium dihydrogen phosphate aluminum;
secondly, adding acetone and a silane coupling agent into the chromium dihydrogen phosphate obtained in the step one, and fully dissolving to obtain a chromium dihydrogen phosphate polymer solution;
adding the polyaluminum carbosilane and the silane coupling agent into an acetone solvent, and fully dissolving to obtain a polyaluminum carbosilane solution;
fourthly, mixing the chromium dihydrogen phosphate polymer solution obtained in the second step with the polyaluminium carbosilane solution obtained in the third step, and stirring to obtain a modified non-aqueous phosphate adhesive matrix;
fifthly, mixing the forsterite sand with the particle size of 120-200 mu m, the magnesia zirconium sand with the particle size of 100-150 mu m, the alumina with the particle size of 10-50 mu m and the alumina with the particle size of 150-200 mu m, dispersing at a high speed, controlling the high temperature of 1350 ℃ for 1h, adding a water reducing agent and a retarder, and dispersing at a high speed again to obtain a curing agent;
sixthly, mixing and stirring the modified non-aqueous phosphate adhesive matrix obtained in the fourth step and the curing agent obtained in the fifth step to form a uniform paste, so as to obtain a phosphate adhesive;
seventhly, putting the quartz fiber cloth with the thickness of 0.1mm into the fiber treating agent for soaking, and then drying; cutting a quartz fiber cloth block with the size of 4-6 mm;
and eighthly, uniformly mixing the quartz fiber cloth block obtained in the seventh step with the phosphate adhesive obtained in the sixth step, putting the mixture into a mould after ramming, and performing vacuum pressurization curing to obtain the heating-free broken block-shaped quartz fiber cloth block reinforced phosphate composite material, thus completing the method.
The working life of the phosphate adhesive obtained in the sixth step is 1 h.
The invention has the beneficial effects that:
the invention has the beneficial effects that: the invention takes normal temperature curing phosphate adhesive, 5mm multiplied by 5mm short cut quartz fiber cloth and silica sol fiber treating agent as main raw materials to prepare a normal temperature curing type quartz fiber reinforced phosphate composite material.
The silica sol fiber treating agent can be converted into silicon dioxide after high-temperature treatment, and has excellent interface bonding performance with quartz fibers, so that the treating agent and the quartz fibers are sintered into a whole under a high-temperature environment, and the mechanical property of the composite material is greatly improved. After the chopped quartz fiber cloth obtained by treatment of the treating agent is compounded and molded with the phosphate adhesive, the chopped quartz fiber cloth is mutually interpenetrated, the interlayer bonding force is improved, and the mechanical property is obviously higher than that of the composite material prepared by the layering process. In addition, the phosphate adhesive is cured at normal temperature, so that the problems of volatilization and corrosion of a vacuum bag, difficult pressure maintaining and the like of a phosphate solvent cured by heating can be solved, the mechanical properties of the prepared composite material heat-resistant quartz fiber cloth reinforced phosphate composite material are equivalent, and the preparation process is simpler.
The method is used for preparing the phosphate composite material.
Detailed Description
The technical solution of the present invention is not limited to the specific embodiments listed below, and includes any combination of the specific embodiments.
The first embodiment is as follows: the embodiment provides a preparation method of a heating-free broken quartz fiber cloth reinforced phosphate composite material, which specifically comprises the following steps:
heating an industrial grade chromium dihydrogen phosphate aluminum solution to obtain a saturated salt solution, controlling the heating temperature to be 78-82 ℃, then cooling to-18-20 ℃, keeping for 12-13 h, crystallizing chromium dihydrogen phosphate aluminum at the bottom, freezing the upper layer, and separating ice to obtain crystallized chromium dihydrogen phosphate aluminum;
secondly, adding acetone and a silane coupling agent into the chromium dihydrogen phosphate obtained in the step one, and fully dissolving to obtain a chromium dihydrogen phosphate polymer solution;
adding the polyaluminum carbosilane and the silane coupling agent into an acetone solvent, and fully dissolving to obtain a polyaluminum carbosilane solution;
fourthly, mixing the chromium dihydrogen phosphate polymer solution obtained in the second step with the polyaluminium carbosilane solution obtained in the third step, and stirring to obtain a modified non-aqueous phosphate adhesive matrix;
fifthly, mixing the forsterite sand with the particle size of 120-200 mu m, the magnesia zirconium sand with the particle size of 100-150 mu m, the alumina with the particle size of 10-50 mu m and the alumina with the particle size of 150-200 mu m, dispersing at a high speed, controlling the high temperature of 1350 ℃ for 1h, adding a water reducing agent and a retarder, and dispersing at a high speed again to obtain a curing agent;
sixthly, mixing and stirring the modified non-aqueous phosphate adhesive matrix obtained in the fourth step and the curing agent obtained in the fifth step to form a uniform paste, so as to obtain a phosphate adhesive;
seventhly, putting the quartz fiber cloth with the thickness of 0.1mm into the fiber treating agent for soaking, and then drying; cutting a quartz fiber cloth block with the size of 4-6 mm;
and eighthly, uniformly mixing the quartz fiber cloth block obtained in the seventh step with the phosphate adhesive obtained in the sixth step, putting the mixture into a mould after ramming, and performing vacuum pressurization curing to obtain the heating-free broken block-shaped quartz fiber cloth block reinforced phosphate composite material, thus completing the method.
The second embodiment is as follows: the first difference between the present embodiment and the specific embodiment is: and step two, by weight, 100 parts of chromium dihydrogen phosphate, 50-150 parts of acetone and 1 part of silane coupling agent. The rest is the same as the first embodiment.
The third concrete implementation mode: the present embodiment differs from the first or second embodiment in that: and step three, according to the weight parts, 2-25 parts of polyaluminum carbosilane, 1 part of silane coupling agent and 100 parts of acetone solvent. The other is the same as in the first or second embodiment.
The fourth concrete implementation mode: the difference between this embodiment mode and one of the first to third embodiment modes is: and step four, 100 parts of the chromium dihydrogen phosphate aluminum polymer solution and 20 parts of the polyaluminium carbosilane solution by weight. The others are the same as in one of the first to third embodiments.
The fifth concrete implementation mode: the difference between this embodiment and one of the first to fourth embodiments is: step five, according to the weight portion, 50 to 100 portions of forsterite sand with the particle size of 120-200 mu m, 10 to 30 portions of magnesium zircon sand with the particle size of 100-150 mu m, 60 to 100 portions of alumina with the particle size of 10 to 50 mu m, 5 to 20 portions of alumina with the particle size of 150 to 200 mu m, 1 portion of water reducing agent and 1 portion of retarder. The other is the same as one of the first to fourth embodiments.
The sixth specific implementation mode: the difference between this embodiment and one of the first to fifth embodiments is: and step six, 100 parts of the modified non-aqueous phosphate adhesive matrix and 80-200 parts of the curing agent by weight. The other is the same as one of the first to fifth embodiments.
The seventh embodiment: the difference between this embodiment and one of the first to sixth embodiments is: and seventhly, the fiber treating agent is polycarbosilane solution, and the soaking time is 2 hours. The other is the same as one of the first to sixth embodiments.
The specific implementation mode is eight: the present embodiment differs from one of the first to seventh embodiments in that: fifthly, the water reducing agent is polycarboxylic acid, and the retarder is a silane coupling agent. The other is the same as one of the first to seventh embodiments.
The specific implementation method nine: the present embodiment differs from the first to eighth embodiments in that: and step eight, 30-60 parts of quartz fiber cloth and 40-70 parts of phosphate adhesive according to the mass parts. The rest is the same as the first to eighth embodiments.
The detailed implementation mode is ten: the present embodiment differs from one of the first to ninth embodiments in that: step eight, vacuum bag is adopted for vacuum pumping, pressurizing and curing, the curing time is 48 hours, and the pressure is 0.08 MPa-0.1 MPa. The other is the same as one of the first to ninth embodiments.
The following examples and comparative experiments were used to verify the beneficial effects of the present invention:
the first embodiment is as follows:
the embodiment of the invention relates to a preparation method of a heating-free broken quartz fiber cloth reinforced phosphate composite material, which specifically comprises the following steps:
heating an industrial grade chromium dihydrogen phosphate aluminum solution to 80 ℃, keeping the temperature for 5 hours to obtain a saturated salt solution, then keeping the saturated salt solution at the temperature of-18 ℃ for 12 hours, crystallizing chromium dihydrogen phosphate aluminum at the bottom, freezing the upper layer, and separating ice to obtain crystallized chromium dihydrogen phosphate aluminum;
secondly, adding 120g of acetone and 1g of silane coupling agent KH560 into 100g of the chromium dihydrogen phosphate obtained in the first step, and fully dissolving to obtain a chromium dihydrogen phosphate polymer solution;
adding 15g of polyaluminum carbosilane and 1g of silane coupling agent into 100g of acetone solvent, and fully dissolving to obtain polyaluminum carbosilane solution;
fourthly, mixing 100g of the chromium dihydrogen phosphate polymer solution obtained in the second step with 20g of the polyaluminium carbosilane solution obtained in the third step, controlling the stirring temperature to be 5 ℃, and stirring for 2 hours to obtain a modified non-aqueous phosphate adhesive matrix;
fifthly, mixing 75g of forsterite sand with the particle size of 160 mu m, 20g of magnesia zirconium sand with the particle size of 125 mu m, 80g of alumina with the particle size of 30 mu m and 12.5g of alumina with the particle size of 170 mu m, dispersing at a high speed for 30min, controlling the temperature at 1350 ℃ for 1h, adding 1g of water reducing agent polycarboxylic acid and 1g of retarder silane coupling agent KH560, and dispersing at a high speed for 30min again to obtain a curing agent; the high-speed dispersion rotating speed is 10000 r/min;
sixthly, mixing and stirring 100g of the modified non-aqueous phosphate adhesive matrix obtained in the fourth step and 140g of the curing agent obtained in the fifth step to form a uniform paste, so as to obtain a phosphate adhesive;
seventhly, putting the quartz fiber cloth with the thickness of 0.1mm into the fiber treating agent, soaking for 2 hours, and then putting the quartz fiber cloth into a drying oven to dry at 60 ℃; then cutting to obtain a quartz fiber cloth block with the size of 5 mm;
eighthly, putting 30g of the quartz fiber cloth block obtained in the first step and 70g of the phosphate adhesive obtained in the sixth step into a barrel, uniformly mixing, ramming for 10 minutes, then putting into a mold, and carrying out vacuum pressurization curing for 48 hours by adopting a vacuum bag to obtain the heating-free broken block-shaped quartz fiber cloth block reinforced phosphate composite material, thereby completing the method.
The bending strength and the interlaminar shear strength of the heating-free broken quartz fiber cloth reinforced phosphate composite material obtained in the embodiment under different temperature conditions are shown in the following table:
test temperature At normal temperature 600℃ 800℃ 1000℃ 1200℃
Strength of bending strength 78MPa 83MPa 74MPa 38MPa 16MPa
Interlaminar shear strength 4.2MPa 4.5MPa 4.0MPa 2.6MPa 2.1MPa
Example two:
the embodiment of the invention relates to a preparation method of a heating-free broken quartz fiber cloth reinforced phosphate composite material, which is different from the first embodiment in that: in the eighth step, 35g of silicon carbide chopped fibers and 65g of phosphate adhesive are used. The rest is the same as the first embodiment.
The bending strength and the interlaminar shear strength of the heating-free broken quartz fiber cloth reinforced phosphate composite material obtained in the embodiment under different temperature conditions are shown in the following table:
test temperature At normal temperature 600℃ 800℃ 1000℃ 1200℃
Strength of bending strength 83MPa 95MPa 89MPa 72MPa 22MPa
Interlaminar shear strength 4.2MPa 5.1MPa 6.4MPa 5.4MPa 3.9MPa
Example three:
the embodiment of the invention relates to a preparation method of a heating-free broken quartz fiber cloth reinforced phosphate composite material, which is different from the first embodiment in that: in the eighth step, 40g of silicon carbide chopped fibers and 60g of phosphate adhesive are used. The rest is the same as the first embodiment.
The method comprises the following steps:
the bending strength and the interlaminar shear strength of the heating-free broken quartz fiber cloth reinforced phosphate composite material obtained in the embodiment under different temperature conditions are shown in the following table:
test temperature At normal temperature 600℃ 800℃ 1000℃ 1200℃
Strength of bending strength 94MPa 97MPa 84MPa 63MPa 46MPa
Interlaminar shear strength 5.3MPa 6.4MPa 6.7MPa 5.8MPa 4.7MPa
Example four:
the embodiment of the invention relates to a preparation method of a heating-free broken quartz fiber cloth reinforced phosphate composite material, which is different from the first embodiment in that: in the eighth step, the amount of the silicon carbide chopped fibers is 45g, and the amount of the phosphate adhesive is 55 g. The rest is the same as the first embodiment.
The bending strength and the interlaminar shear strength of the heating-free broken quartz fiber cloth reinforced phosphate composite material obtained in the embodiment under different temperature conditions are shown in the following table:
test temperature At normal temperature 600℃ 800℃ 1000℃ 1200℃
Strength of bending strength 98MPa 103MPa 87MPa 56MPa 54MPa
Interlaminar shear strength 6.2MPa 6.4MPa 6.3MPa 6.4MPa 6.5MPa
Example five:
the embodiment of the invention relates to a preparation method of a heating-free broken quartz fiber cloth reinforced phosphate composite material, which is different from the first embodiment in that: in the eighth step, 50g of silicon carbide chopped fibers and 50g of phosphate adhesive are used. The rest is the same as the first embodiment.
The bending strength and the interlaminar shear strength of the heating-free broken quartz fiber cloth reinforced phosphate composite material obtained in the embodiment under different temperature conditions are shown in the following table:
test temperature At normal temperature 600℃ 800℃ 1000℃ 1200℃
Strength of bending strength 123MPa 115MPa 98MPa 67MPa 54MPa
Interlaminar shear strength 7.5MPa 7.7MPa 7.3MPa 6.5MPa 5.3MPa
Example six:
the embodiment relates to a preparation method of a heating-free broken quartz fiber cloth reinforced phosphate composite material,
the difference from the first embodiment is that: in the eighth step, 55g of silicon carbide chopped fibers and 45g of phosphate adhesive are adopted. The rest is the same as the first embodiment.
The bending strength and the interlaminar shear strength of the heating-free broken quartz fiber cloth reinforced phosphate composite material obtained in the embodiment under different temperature conditions are shown in the following table:
test temperature At normal temperature 600℃ 800℃ 1000℃ 1200℃
Strength of bending strength 165MPa 137MPa 126MPa 96MPa 34MPa
Interlaminar shear strength 7.6MPa 8.1MPa 6.5MPa 6.4MPa 5.5MPa
Example seven:
the embodiment of the invention relates to a preparation method of a heating-free broken quartz fiber cloth reinforced phosphate composite material, which is different from the first embodiment in that: in the eighth step, 60g of silicon carbide chopped fibers and 40g of phosphate adhesive are used. The rest is the same as the first embodiment.
The bending strength and the interlaminar shear strength of the heating-free broken quartz fiber cloth reinforced phosphate composite material obtained in the embodiment under different temperature conditions are shown in the following table:
Figure BDA0003099334590000061
Figure BDA0003099334590000071
the composite materials obtained by the first to seventh embodiments have simple preparation process, do not need heating, are more energy-saving, are disordered, interpenetrated and dispersed in the composite materials, are sintered into a whole by the quartz fibers and the silica sol treating agent after high-temperature treatment, have higher interlayer bonding force, have excellent normal-temperature and high-temperature bending properties, and meet the use requirements.

Claims (10)

1. A preparation method of a heating-free broken quartz fiber cloth reinforced phosphate composite material is characterized by comprising the following steps:
heating an industrial grade chromium dihydrogen phosphate aluminum solution to obtain a saturated salt solution, controlling the heating temperature to be 78-82 ℃, then cooling to-18-20 ℃, keeping for 12-13 h, crystallizing chromium dihydrogen phosphate aluminum at the bottom, freezing the upper layer, and separating ice to obtain crystallized chromium dihydrogen phosphate aluminum;
secondly, adding acetone and a silane coupling agent into the chromium dihydrogen phosphate obtained in the step one, and fully dissolving to obtain a chromium dihydrogen phosphate polymer solution;
adding the polyaluminum carbosilane and the silane coupling agent into an acetone solvent, and fully dissolving to obtain a polyaluminum carbosilane solution;
fourthly, mixing the chromium dihydrogen phosphate polymer solution obtained in the second step with the polyaluminium carbosilane solution obtained in the third step, and stirring to obtain a modified non-aqueous phosphate adhesive matrix;
fifthly, mixing the forsterite sand with the particle size of 120-200 mu m, the magnesia zirconium sand with the particle size of 100-150 mu m, the alumina with the particle size of 10-50 mu m and the alumina with the particle size of 150-200 mu m, dispersing at a high speed, controlling the high temperature of 1350 ℃ for 1h, adding a water reducing agent and a retarder, and dispersing at a high speed again to obtain a curing agent;
sixthly, mixing and stirring the modified non-aqueous phosphate adhesive matrix obtained in the fourth step and the curing agent obtained in the fifth step to form a uniform paste, so as to obtain a phosphate adhesive;
seventhly, putting the quartz fiber cloth with the thickness of 0.1mm into the fiber treating agent for soaking, and then drying; cutting a quartz fiber cloth block with the size of 4-6 mm;
and eighthly, uniformly mixing the quartz fiber cloth block obtained in the seventh step with the phosphate adhesive obtained in the sixth step, putting the mixture into a mould after ramming, and performing vacuum pressurization curing to obtain the heating-free broken block-shaped quartz fiber cloth block reinforced phosphate composite material, thus completing the method.
2. The preparation method of the heating-free broken quartz fiber cloth reinforced phosphate composite material according to claim 1, wherein in the second step, 100 parts of chromium dihydrogen phosphate, 50-150 parts of acetone and 1 part of silane coupling agent are used according to parts by weight.
3. The preparation method of the heating-free broken quartz fiber cloth reinforced phosphate composite material according to claim 1, wherein in the third step, 2-25 parts of polyaluminum carbosilane, 1 part of silane coupling agent and 100 parts of acetone solvent are used according to parts by weight.
4. The preparation method of the heating-free broken quartz fiber cloth reinforced phosphate composite material as claimed in claim 1, wherein in the fourth step, the chromium dihydrogen phosphate polymer solution is 100 parts by weight, and the polyaluminium carbosilane solution is 20 parts by weight.
5. The preparation method of the heating-free broken quartz fiber cloth reinforced phosphate composite material as claimed in claim 1, wherein the step five comprises, by weight, 50-100 parts of 200 μm forsterite sand with a particle size of 120-.
6. The preparation method of the heating-free broken quartz fiber cloth reinforced phosphate composite material according to claim 1, wherein in the sixth step, 100 parts of the modified non-aqueous phosphate adhesive matrix and 80-200 parts of the curing agent are used by weight.
7. The method for preparing the heating-free broken quartz fiber cloth reinforced phosphate composite material according to claim 1, wherein the fiber treating agent in the seventh step is polycarbosilane solution, and the soaking time is 2 hours.
8. The preparation method of the heating-free broken quartz fiber cloth reinforced phosphate composite material according to claim 1, wherein the water reducing agent in the step five is polycarboxylic acid, and the retarder is a silane coupling agent.
9. The preparation method of the heating-free broken quartz fiber cloth reinforced phosphate composite material according to claim 1, wherein in the eighth step, 30-60 parts by weight of quartz fiber cloth and 40-70 parts by weight of phosphate adhesive are used.
10. The preparation method of the heating-free broken quartz fiber cloth reinforced phosphate composite material according to claim 1, wherein in the eighth step, vacuum bag is adopted for vacuum pumping and pressurizing curing, the curing time is 48h, and the pressure is 0.08MPa to 0.1 MPa.
CN202110620473.1A 2021-06-03 2021-06-03 Preparation method of heating-free broken quartz fiber cloth reinforced phosphate composite material Active CN113321483B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202110620473.1A CN113321483B (en) 2021-06-03 2021-06-03 Preparation method of heating-free broken quartz fiber cloth reinforced phosphate composite material

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202110620473.1A CN113321483B (en) 2021-06-03 2021-06-03 Preparation method of heating-free broken quartz fiber cloth reinforced phosphate composite material

Publications (2)

Publication Number Publication Date
CN113321483A true CN113321483A (en) 2021-08-31
CN113321483B CN113321483B (en) 2023-02-03

Family

ID=77419550

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202110620473.1A Active CN113321483B (en) 2021-06-03 2021-06-03 Preparation method of heating-free broken quartz fiber cloth reinforced phosphate composite material

Country Status (1)

Country Link
CN (1) CN113321483B (en)

Citations (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5371050A (en) * 1989-08-14 1994-12-06 Aluminum Company Of America Aluminum phosphate bonded fiber reinforced composite material containing metal coated fibers
JPH07196374A (en) * 1993-12-29 1995-08-01 Tonen Corp Prepreg for fiber-reinforced ceramic and its application
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
CN102807353A (en) * 2012-08-29 2012-12-05 黑龙江省科学院石油化学研究院 Method for preparing quartz fiber reinforced phosphate-based high temperature resistant composite material
CN102910928A (en) * 2012-11-13 2013-02-06 黑龙江省科学院石油化学研究院 Preparation method of phosphate base composite material resistant to superhigh temperature of 1700 DEG C
CN103468154A (en) * 2013-08-27 2013-12-25 黑龙江省科学院石油化学研究院 High-temperature-resistant room temperature curing phosphate adhesive and preparation method thereof
CN103880436A (en) * 2014-01-26 2014-06-25 黑龙江省科学院石油化学研究院 Preparation method of 1500 DEG C resistant heat insulating layer material
CN103936390A (en) * 2014-02-21 2014-07-23 湖北三江航天江北机械工程有限公司 Preparation method of phosphate composite material radome body
CN105174899A (en) * 2015-09-06 2015-12-23 东南大学 Phosphate-based composite material and preparation method thereof
CN105802516A (en) * 2016-06-03 2016-07-27 黑龙江省科学院石油化学研究院 Preparation method of alcohol-soluble high-temperature-resistant phosphate adhesive
CN106242550A (en) * 2016-07-22 2016-12-21 哈尔滨工业大学 A kind of moistureproof wave transparent quartz fibre/phosphate ceramics composite material and preparation method thereof
CN108794046A (en) * 2018-07-11 2018-11-13 航天材料及工艺研究所 A kind of alumina ceramic-base composites honeycomb and preparation method thereof
CN110256091A (en) * 2019-06-24 2019-09-20 湖北三江航天江北机械工程有限公司 Polycrystalline mullite fibre enhances the efficient forming method of phosphate composite ceramics antenna house
CN113264753A (en) * 2021-06-03 2021-08-17 哈尔滨工程大学 Preparation method of heating-free short silicon carbide fiber reinforced phosphate composite material

Patent Citations (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5371050A (en) * 1989-08-14 1994-12-06 Aluminum Company Of America Aluminum phosphate bonded fiber reinforced composite material containing metal coated fibers
JPH07196374A (en) * 1993-12-29 1995-08-01 Tonen Corp Prepreg for fiber-reinforced ceramic and its application
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
CN102807353A (en) * 2012-08-29 2012-12-05 黑龙江省科学院石油化学研究院 Method for preparing quartz fiber reinforced phosphate-based high temperature resistant composite material
CN102910928A (en) * 2012-11-13 2013-02-06 黑龙江省科学院石油化学研究院 Preparation method of phosphate base composite material resistant to superhigh temperature of 1700 DEG C
CN103468154A (en) * 2013-08-27 2013-12-25 黑龙江省科学院石油化学研究院 High-temperature-resistant room temperature curing phosphate adhesive and preparation method thereof
CN103880436A (en) * 2014-01-26 2014-06-25 黑龙江省科学院石油化学研究院 Preparation method of 1500 DEG C resistant heat insulating layer material
CN103936390A (en) * 2014-02-21 2014-07-23 湖北三江航天江北机械工程有限公司 Preparation method of phosphate composite material radome body
CN105174899A (en) * 2015-09-06 2015-12-23 东南大学 Phosphate-based composite material and preparation method thereof
CN105802516A (en) * 2016-06-03 2016-07-27 黑龙江省科学院石油化学研究院 Preparation method of alcohol-soluble high-temperature-resistant phosphate adhesive
CN106242550A (en) * 2016-07-22 2016-12-21 哈尔滨工业大学 A kind of moistureproof wave transparent quartz fibre/phosphate ceramics composite material and preparation method thereof
CN108794046A (en) * 2018-07-11 2018-11-13 航天材料及工艺研究所 A kind of alumina ceramic-base composites honeycomb and preparation method thereof
CN110256091A (en) * 2019-06-24 2019-09-20 湖北三江航天江北机械工程有限公司 Polycrystalline mullite fibre enhances the efficient forming method of phosphate composite ceramics antenna house
CN113264753A (en) * 2021-06-03 2021-08-17 哈尔滨工程大学 Preparation method of heating-free short silicon carbide fiber reinforced phosphate composite material

Non-Patent Citations (9)

* Cited by examiner, † Cited by third party
Title
张彬主编: "《混凝土与砂浆配合比手册》", 30 November 2012, 天津大学出版社 *
曹先启等: "聚碳硅烷含量对杂化磷酸盐胶黏剂性能的影响", 《化学与黏合》 *
杨连等: "功能化碳化硅纤维研究进展", 《人工晶体学报》 *
王勃等: "聚碳硅烷对磷酸盐胶黏剂性能影响", 《化学与黏合》 *
祖群等: "《高性能玻璃纤维》", 31 July 2017, 国防工业出版社 *
范叶明等: "几种新型陶瓷天线罩材料与制备工艺", 《热处理技术与装备》 *
谢丽娜等: "陶质文物无机胶黏剂研究", 《南阳理工学院学报》 *
贺曼罗编著: "《建筑胶粘剂》", 30 September 1999, 化学工业出版社 *
陈洋等: "高温黏结剂的研究进展", 《耐火材料》 *

Also Published As

Publication number Publication date
CN113321483B (en) 2023-02-03

Similar Documents

Publication Publication Date Title
CN110790530B (en) High-strength nano heat-insulating material and preparation method thereof
CN110627517B (en) Gradient ultrahigh-temperature ceramic matrix composite material and preparation method thereof
CN110498685B (en) Preparation method of carbon fiber reinforced ceramic matrix composite
CN102146196B (en) Preparation method of high damping epoxy resin composite
CN108892523B (en) Preparation method of carbon-ceramic composite material based on unidirectional tape process
CN107032826B (en) Preparation method of hollow alumina ball/silicon carbide reinforced copper-based composite material
CN110951103A (en) Carbon fiber reinforced phenolic aerogel composite material, preparation method thereof and carbon fiber reinforced carbon aerogel composite material
CN111517770A (en) Production method of high-compactness fused quartz ceramic
CN113264753B (en) Preparation method of heating-free short silicon carbide fiber reinforced phosphate composite material
CN111908932A (en) Light efficient heat-insulation integrated thermal protection material and preparation method thereof
CN104529499A (en) Preparation method of self-healing silicon-carbide-fiber-reinforced silicon-boron-nitrogen-carbon composite material
CN109437813A (en) Low temperature cold fires the method and its ceramic application of standby inorganic polymer composite material
CN114262179B (en) Mullite fiber reinforced geopolymer composite material and preparation method and application thereof
CN113321483B (en) Preparation method of heating-free broken quartz fiber cloth reinforced phosphate composite material
CN110040995B (en) Preparation method of high-temperature light tough mullite aggregate
CN113651627B (en) Preparation method and application of alumina fiber reinforced alumina ceramic matrix composite
CN108793911B (en) Method for preparing magnesium lightweight aggregate by foaming method
CN113754455A (en) Multi-scale toughening layer structure wave-absorbing ceramic matrix composite and preparation method thereof
CN113831102B (en) Continuous basalt fiber reinforced phosphate group geopolymer composite material and preparation method thereof
CN113185921B (en) Preparation method of ceramic precursor modified phosphate adhesive
CN115259876A (en) Preparation method of homogeneous mullite fiber-based porous ceramic
CN112500181B (en) Silica short fiber mould pressing ceramic antenna window composite material and preparation method thereof
CN112174651B (en) Light refractory brick and preparation method thereof
CN111908842A (en) Nano heat-insulating material and preparation method thereof
CN112645713A (en) High-toughness ceramic composite material and preparation method thereof

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant