CN105419720A - Nano particle modified binder, preparation method and using method - Google Patents
Nano particle modified binder, preparation method and using method Download PDFInfo
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- CN105419720A CN105419720A CN201510919082.4A CN201510919082A CN105419720A CN 105419720 A CN105419720 A CN 105419720A CN 201510919082 A CN201510919082 A CN 201510919082A CN 105419720 A CN105419720 A CN 105419720A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 20
- 239000002105 nanoparticle Substances 0.000 title abstract description 9
- 239000000843 powder Substances 0.000 claims abstract description 39
- 238000010438 heat treatment Methods 0.000 claims abstract description 17
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- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910052580 B4C Inorganic materials 0.000 claims abstract description 12
- INAHAJYZKVIDIZ-UHFFFAOYSA-N boron carbide Chemical compound B12B3B4C32B41 INAHAJYZKVIDIZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000005229 chemical vapour deposition Methods 0.000 claims abstract description 5
- 239000000126 substance Substances 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 claims description 35
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 30
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical group CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 24
- 229920002050 silicone resin Polymers 0.000 claims description 24
- 238000003756 stirring Methods 0.000 claims description 22
- 238000011049 filling Methods 0.000 claims description 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- 239000007822 coupling agent Substances 0.000 claims description 16
- 229910052782 aluminium Inorganic materials 0.000 claims description 14
- 239000004411 aluminium Substances 0.000 claims description 14
- 238000002156 mixing Methods 0.000 claims description 14
- 230000010355 oscillation Effects 0.000 claims description 14
- 229910021487 silica fume Inorganic materials 0.000 claims description 14
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 10
- 239000003960 organic solvent Substances 0.000 claims description 10
- 238000007669 thermal treatment Methods 0.000 claims description 10
- 230000004048 modification Effects 0.000 claims description 9
- 238000012986 modification Methods 0.000 claims description 9
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 238000009413 insulation Methods 0.000 claims description 8
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000000151 deposition Methods 0.000 claims description 6
- 230000008021 deposition Effects 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 6
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 6
- DPQUFPIZKSPOIF-UHFFFAOYSA-N methane propane Chemical compound C.CCC.CCC DPQUFPIZKSPOIF-UHFFFAOYSA-N 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 5
- 230000008569 process Effects 0.000 claims description 5
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 claims description 5
- 235000019982 sodium hexametaphosphate Nutrition 0.000 claims description 5
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 claims description 5
- 244000137852 Petrea volubilis Species 0.000 claims description 4
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 4
- 239000012298 atmosphere Substances 0.000 claims description 4
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- 239000011347 resin Substances 0.000 abstract description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract 1
- 229910052710 silicon Inorganic materials 0.000 abstract 1
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- HPNSNYBUADCFDR-UHFFFAOYSA-N chromafenozide Chemical compound CC1=CC(C)=CC(C(=O)N(NC(=O)C=2C(=C3CCCOC3=CC=2)C)C(C)(C)C)=C1 HPNSNYBUADCFDR-UHFFFAOYSA-N 0.000 description 6
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- 230000001070 adhesive effect Effects 0.000 description 4
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- 239000013590 bulk material Substances 0.000 description 3
- 239000002086 nanomaterial Substances 0.000 description 3
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- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 1
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- 238000007711 solidification Methods 0.000 description 1
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- Compositions Of Macromolecular Compounds (AREA)
- Adhesives Or Adhesive Processes (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention relates to a nano particle modified binder which comprises a binder main body and nanofiller, wherein the binder main body comprises 45-55 wt% of organic silicon resin, 25-35 wt% of glass powder and 15-20 wt% of boron carbide powder; and the nanofiller comprises 5-10 wt% of nanometer aluminum powder, 5-10 wt% of nanometer silica powder and 1-2 wt% of alumina whisker. A method for preparing the nano particle modified binder comprises the steps of respectively preparing the binder main body and the nanofiller and then evenly dispersing and adding the nanofiller in the binder main body. A method for using the binder comprises the steps of evenly bonding the to-be-glued surface of an object with the binder, bonding the object, and achieving object bonding after heat treatment and chemical vapor deposition. The binder accord to the preparation method and the using method not only is extensive in use range, but also has good heat resistance and keeps physical and chemical properties basically unchanged in high temperature environment for a long time.
Description
Technical field
The present invention relates to high temperature bond technical field, particularly relate to a kind of nanometer particle-modified binding agent, preparation method and using method.
Background technology
Silicone resin is with the performance of its excellence, in widespread attention in high temperature structural composite material bonding field.Silicone backbone is Si-O-Si key, have very high bond energy and ion tendency, side chain is organic group, thus has organic and feature that is inorganic materials concurrently, not only there is excellent resistance toheat, and its physicochemical property can be kept within the scope of 60 ~ 1200 DEG C substantially constant.But silicone resin is crisp, cohesive strength is low, solidification value is high, therefore need in use procedure to carry out modification.In silicone resin, content inorganic filling polymkeric substance then can carry out modification to silicone resin, and inorganics polymkeric substance effectively can alleviate the internal stress that volumetric shrinkage causes, and improves binding agent intensity at high temperature.But fill while inorganic polymer improves rigidity of material and can reduce its toughness.
By the characteristic of nano material and experimental studies have found that, add nano material and the rigidity that modification can not only improve material is carried out to silicone resin, the toughness of material can be improved simultaneously.Nanoparticle can disperse uniformly in resin matrix, when resin matrix is subject to impacting, the existence of rigidity nanoparticle is easy to produce concentration effect and make its surrounding matrix resin produce crazing, matrix simultaneously between particle also produces viscous deformation, crazing and viscous deformation can absorb striking energy on the one hand, rigidity nanoparticle makes crazing be obstructed or passivation on the other hand, reaches the effect increasing toughness.Along with diminishing of nano-particles size, the specific surface area of particle increases, and the interface of particle and matrix becomes greatly, and crazing and the viscous deformation of generation are larger, thus absorb more striking energy, and increasing toughness effect will improve.If therefore by nano material admixture in a binder, while guarantee toughness effect, can realize high temperature cohesive strength will be huge technical progress.
Summary of the invention
In view of above-mentioned analysis, the present invention aims to provide a kind of nanometer particle-modified binding agent, preparation method and using method, this binding agent use range is wide, can be bondd of the same race or foreign material, not only cohesive strength is large, resistance toheat is good, physicochemical property can be kept substantially constant in long-time hot environment simultaneously.
Object of the present invention is mainly achieved through the following technical solutions:
A kind of nanometer particle-modified binding agent of the present invention, comprise binding agent main body and Nano filling, it is characterized in that, described binding agent main body comprises: silicone resin 45-55wt.%, glass powder 25-35wt.% and boron carbide powder 15-20wt.%; Described Nano filling comprises: to account for the part by weight of described binding agent main body, nanometer aluminium powder 5-10wt.%, nano silica fume 5-10wt.% and alumina whisker 1-2wt.%.
Further, described glass powder, granularity is 400 ~ 500 orders, and fusing point is 400 ~ 500 DEG C;
Described boron carbide powder, granularity is 225 ~ 300 orders.
The preparation method of a kind of nanometer particle-modified binding agent of the present invention, comprises the preparation of binding agent main body, Nano filling preparation and the nano modification of binding agent:
(1) binding agent main body preparation: take a certain amount of binding agent host component by the dosage principle of binding agent host component, described silicone resin is put into wide neck flask, and add the organic solvent with described silicone resin equivalent, heating in water bath, stirring, until described silicone resin all dissolves, wherein, during described heating in water bath, constantly in wide neck flask, instill described organic solvent, be as the criterion just to keep solution mobility in wide-necked bottle; Then described glass powder and described boron carbide powder are added in described wide neck flask and stir 1 ~ 3 hour, constantly the described organic solvent of instillation, makes all substances in described wide neck flask mix completely, and ensures mobility, be then placed in ventilation and store for future use;
(2) Nano filling preparation: take a certain amount of nanofiller component by the dosage principle of nanofiller component, described nanometer aluminium powder and nano silica fume being put into deionized water makes it mix formation mixing solutions, add account for described mixing solutions weight 0.5wt.% Sodium hexametaphosphate 99 as dispersion agent, prevent from producing sedimentation and cohesion in nanometer aluminium powder and nano silica fume mixing process, ensure good homogeneity, then stirring at normal temperature 1 hour, sonic oscillation post-drying are for subsequent use; Described alumina whisker is put into deionized water, and adds coupling agent solution, sonic oscillation post-drying is for subsequent use;
(3) nano modification of binding agent: Nano filling prepared by described step (2) is joined in the binding agent main body of described step (1), heating in water bath, stirring and the described organic solvent of continuous instillation, after 1 ~ 3 hour, stop adding solvent, continuation heating in water bath and stirring are until solution becomes sticky thick, by the state that glass stick can just be provoked, described binding agent is ready to complete.
Further, described coupling agent solution is: coupling agent adds in ethanol-water solution, and accounting for ethanol-water solution weight percent according to coupling agent is that the proportioning of 0.2wt.% ~ 1wt.% mixes, and regulates pH to be 5.5 ~ 6.5; In wherein said ethanol-water solution, ethanol and water ratio are 1:1 ~ 2:1, and described coupling agent is silane coupling agent KH-540.
Further, organic solvent described in described step (1) and described step (3) is dimethylbenzene.
Further, step (1) and step (3) water bath heating temperature are 60 DEG C, and described step (2) described sonic oscillation is 30min, and described bake out temperature is 80 DEG C.
The using method of a kind of nanometer particle-modified binding agent of the present invention, is characterized in that, comprises the step that object bonding, thermal treatment and CVI (ChemicalVaporInfiltration) deposit:
(1) object bonding: sand paper polishes evenly cutting after to be bonded of object, and described groove depth is 0.5mm, and in alcohol sonic oscillation post-drying, then be applied on to be bonded by even for described binding agent, the docking of to be bonded of two articles, bubble is got rid of in the left and right changing of the relative positions simultaneously, fixes with fixture; Described groove can increase matrix surface hole or concave surface, described binding agent infiltrates hole or concave surface, forms various forms of engaging structure on the one hand in interface region, forms " chock " on the other hand and is pinned in bulk material, increase bonding strength;
(2) thermal treatment: object after bonding is put into process furnace, with ramp to the 200 DEG C insulation 2 hours of 5 DEG C/min ~ 10 DEG C/min under protective atmosphere, then with ramp to the 1000 DEG C insulation 2 hours of 5 DEG C/min ~ 10 DEG C/min;
(3) CVI deposition: the described object after thermal treatment puts into chemical vapor deposition stove, passes into methane-propane mixture body, and control temperature is 1000 ~ 1500 DEG C, and pressure range is 2K ~ 5KPa, carries out vapour deposition.
Further, the described protective atmosphere in step (2) is argon gas, and flow is 50ml/min ~ 100ml/min.
Further, in described methane-propane mixture body, methane and propane volume ratio are 1:1 ~ 3:1.
Beneficial effect of the present invention is as follows:
The nanometer particle-modified binding agent of one provided by the invention, carrying out modified organic silicone resin matrix by filling the nanoparticle such as nanometer aluminium powder and nano silica fume in silicone resin, improving the rigidity of material, toughness and high temperature cohesive strength simultaneously.Binding agent use range of the present invention is wide, and not only can bond carbon based material of the same race and ceramic based material etc., foreign material can be bonded together simultaneously; Binding agent resistance toheat of the present invention is good, and physicochemical property can be kept in long-time hot environment substantially constant, and under 800 DEG C of environment, after 100 hours, mechanical property is substantially constant.
Other features and advantages of the present invention will be set forth in the following description, and, becoming apparent from specification sheets of part, or understand by implementing the present invention.Object of the present invention and other advantages are by realizing at write specification sheets, claims and obtain.
Embodiment
Below in conjunction with preferred embodiment, technical scheme of the present invention is described in further detail, should be appreciated that following examples only for explaining and the present invention being described, but do not form the restriction to technical solution of the present invention.
Silicone resin of the present invention is tetraethyl orthosilicate, is industrial standards;
Described glass powder, granularity is 400 ~ 500 orders, and fusing point is 400 ~ 500 DEG C, is industrial standards;
Described boron carbide powder, granularity is 225 ~ 300 orders, is analytical pure standard;
Described nanometer aluminium powder, median size is 50nm, and purity is 99.5%;
Described nano silica fume, median size is 35nm, and purity is 99.9%;
Described alumina whisker, mean diameter is 100nm, and mean length is 50 μm;
Described dimethylbenzene, Sodium hexametaphosphate 99, methane and propane are analytical pure standard;
Described argon gas is industrial standards.
Embodiment 1
The nanometer particle-modified binding agent of one prepared by the present invention, wherein binding agent main body comprises silicone resin 55wt.%, glass powder 30wt.% and boron carbide powder 15wt.%, wherein Nano filling comprises: nanometer aluminium powder 10wt.%, nano silica fume 10wt.% and alumina whisker 1wt.%.
The preparation method of this binding agent, comprises the following steps:
1) binding agent main body preparation: take 55wt.% silicone resin and put into wide neck flask, add with the dimethylbenzene of silicone resin equivalent as solvent, carry out 60 DEG C of heating in water bath, stirring, during heating in water bath, in wide-necked bottle, constantly instillation dimethylbenzene is as the criterion just to ensure in wide neck flask that liquid can flow; Then take 30wt.% glass powder and 15wt.% boron carbide powder to add in described wide neck flask and stir 2 hours, make it mix completely, period constantly instills the mobility that dimethylbenzene ensures described binding agent main body, is then placed in ventilation and stores for future use;
(2) Nano filling preparation: take the nanometer aluminium powder of the 10wt.% accounting for binding agent main body gross weight and 10wt.% nano silica fume and put into deionized water for stirring and evenly form mixing solutions, then add account for described mixing solutions weight 0.5wt.% Sodium hexametaphosphate 99 as dispersion agent, prevent from producing sedimentation and cohesion in nanometer aluminium powder and nano silica fume mixing process, ensure good homogeneity, then after stirring at normal temperature 1 hour, sonic oscillation 30min, in 80 DEG C of dry for standby; Silane coupling agent KH-540 is joined ethanol and water ratio is dilute in the mixing solutions of 1:1, the mixing solutions weight percent making coupling agent account for ethanol and water is 0.3wt.%, regulator solution pH is 6.5, obtained coupling agent solution, then take the alumina whisker accounting for binding agent main body gross weight 1wt.% to mix with deionized water, and add described coupling agent solution, after sonic oscillation 30min, in 80 DEG C of dry for standby;
(3) nano modification of binding agent: Nano filling prepared by step (2) is joined in the binding agent main body of described step (1), 60 DEG C of heating in water bath, stirring, period constantly instills xylene solvent, after 2 hours, stop adding dimethylbenzene, continuation water-bath and stirring are until solution becomes sticky thick, and the state can just provoked with glass stick, completes binding agent preparation.
The described nanometer particle-modified binding agent of preparation is used for the bonding of object, its using method comprises the following steps:
(1) object bonding: polishing rear even quarter by be bonded for object with 200 order SiC sand paper is the groove of 0.5mm deeply, sonic oscillation in alcohol is also dried, be applied to be bonded by even for the binding agent of preparation, after object bonding, bubble is got rid of in the left and right changing of the relative positions, fixes with graphite fixture; Described groove can increase matrix surface hole or concave surface, described binding agent infiltrates hole or concave surface, and form various forms of engaging structure in interface region, the interfacial mechanical reactive force produced therefrom plays a very important role to cohesive strength; In addition due to the existence of groove certain roughness that made surface have, binding agent flows into and displaces the air of the inside, object so to be bonded just can along bending path close contact, be equivalent to hammer in bulk material one " chock ", play the effect of good physics pinning, therefore the expansion approach of crackle is also distorted, turn in tack coat, tack coat generation viscous deformation, consumes a large amount of energy, thus makes adhesive strength show get Geng Gao;
(2) thermal treatment: put into tube furnace after object bonding, with the ramp to 200 of 5 DEG C/min DEG C insulation 2 hours under argon atmosphere, then continue within 2 hours, to heat-treat with DEG C insulation of the ramp to 1000 of 5 DEG C/min, wherein argon flow amount is 50ml/min;
(3) CVI deposition: put into chemical vapor deposition stove after object thermal treatment, passing into methane-propane volume ratio is the mixed gas of 1:1, and control temperature is 1500 DEG C, and pressure is 2K.
Performance test after the binding agent use that embodiment 1 is prepared, carry out as follows:
(1) adhesive property test, on universal electrical sample machine, the cutting performance of test sample reaches 11Mpa, and the failure mode of object is mixed fracture, illustrates that the intensity of tack coat meets service requirements.
(2) resistance toheat test, puts into tube furnace by the object after bonding, under argon atmosphere, be incubated 100 hours at 800 DEG C, and then being naturally cooled to room temperature, to test its cohesive strength be 7.2Mpa.
(3) use range test, same type of material bonds: based composite material of carbon/based composite material of carbon, ceramic matric composite/ceramic matric composite; Foreign material bonds: based composite material of carbon/ceramic matric composite; Test its shearing resistance, all meet service requirements.
Embodiment 2
The nanometer particle-modified binding agent of one prepared by the present invention, wherein binding agent main body comprises silicone resin 50wt.%, glass powder 35wt.% and boron carbide powder 15wt.%, wherein Nano filling comprises: nanometer aluminium powder 5wt.%, nano silica fume 5wt.% and alumina whisker 2wt.%.
The preparation method of this binding agent, comprises the following steps:
1) binding agent main body preparation: take 50wt.% silicone resin and put into wide neck flask, add with the dimethylbenzene of silicone resin equivalent as solvent, carry out 60 DEG C of heating in water bath, stirring, during heating in water bath, in wide-necked bottle, constantly instillation dimethylbenzene is as the criterion just to ensure in wide neck flask that liquid can flow; Then take 35wt.% glass powder and take 15wt.% boron carbide powder add in described wide neck flask stir 2 hours, make it mix completely, period constantly instills the mobility that dimethylbenzene ensures described binding agent main body, is then placed in ventilation and stores for future use;
(2) Nano filling preparation: take the nanometer aluminium powder of the 5wt.% accounting for binding agent main body gross weight and 5wt.% nano silica fume and put into deionized water for stirring and evenly form mixing solutions, then add account for described mixing solutions weight 0.5wt.% Sodium hexametaphosphate 99 as dispersion agent, prevent from producing sedimentation and cohesion in nanometer aluminium powder and nano silica fume mixing process, ensure good homogeneity, then after stirring at normal temperature 1 hour, sonic oscillation 30min, in 80 DEG C of dry for standby; Silane coupling agent KH-540 is joined ethanol and water ratio is dilute in the mixing solutions of 1.5:1, coupling agent is made to account for ethanol and water mixed solution weight percent is 1wt.%, regulator solution pH is 5.5, obtained coupling agent solution, then take the alumina whisker accounting for binding agent main body gross weight 2wt.% to mix with deionized water, and add described coupling agent solution, after sonic oscillation 30min, in 80 DEG C of dry for standby;
(3) nano modification of binding agent: Nano filling prepared by step (2) is joined in the binding agent main body of described step (1), 60 DEG C of heating in water bath, stirring, period constantly instills xylene solvent, after 2 hours, stop adding dimethylbenzene, continuation water-bath and stirring are until solution becomes sticky thick, and the state can just provoked with glass stick, completes binding agent preparation.
The described nanometer particle-modified binding agent of preparation is used for the bonding of object, its using method comprises the following steps:
(1) object bonding: polishing rear even quarter by be bonded for object with 200 order SiC sand paper is the groove of 0.5mm deeply, sonic oscillation in alcohol is also dried, be applied to be bonded by even for the binding agent of preparation, after object bonding, bubble is got rid of in the left and right changing of the relative positions, fixes with graphite fixture; Described groove can increase matrix surface hole or concave surface, described binding agent infiltrates hole or concave surface, and form various forms of engaging structure in interface region, the interfacial mechanical reactive force produced therefrom plays a very important role to cohesive strength; In addition due to the existence of groove certain roughness that made surface have, binding agent flows into and displaces the air of the inside, object so to be bonded just can along bending path close contact, be equivalent to hammer in bulk material one " chock ", play the effect of good physics pinning, therefore the expansion approach of crackle is also distorted, turn in tack coat, tack coat generation viscous deformation, consumes a large amount of energy, thus makes adhesive strength show get Geng Gao;
(2) thermal treatment: put into tube furnace after object bonding, with the ramp to 200 of 10 DEG C/min DEG C insulation 2 hours under argon atmosphere, then continue within 2 hours, to heat-treat with DEG C insulation of the ramp to 1000 of 10 DEG C/min, wherein argon flow amount is 100ml/min;
(3) CVI deposition: put into chemical vapor deposition stove after thermal treatment, passing into methane-propane volume ratio is the mixed gas of 3:1, and control temperature is 1000 DEG C, and pressure is 5K.
Performance test after the binding agent use that embodiment 2 is prepared, carry out as follows:
(1) adhesive property test, on universal electrical sample machine, the cutting performance of test sample reaches 12.6Mpa, and the failure mode of object is base fracture, illustrates that the intensity of tack coat meets service requirements.
(2) resistance toheat test, puts into tube furnace by the object after bonding, under argon atmosphere, be incubated 100 hours at 800 DEG C, and then being naturally cooled to room temperature, to test its cohesive strength be 8.0Mpa.
(3) use range test, same type of material bonds: based composite material of carbon/based composite material of carbon, ceramic matric composite/ceramic matric composite; Foreign material bonds: based composite material of carbon/ceramic matric composite; Test its shearing resistance, all meet service requirements.
In sum, embodiments provide a kind of nanometer particle-modified binding agent, preparation method and using method, modified organic silicone resin matrix is carried out by filling the nanoparticle such as nanometer aluminium powder and nano silica fume in silicone resin, improve the rigidity of material, toughness and high temperature cohesive strength simultaneously, not only use range is extensive, keeps the performance that physicochemical property is substantially constant under having good resistance toheat and long-time hot environment simultaneously.
The above; be only the present invention's preferably embodiment, but protection scope of the present invention is not limited thereto, is anyly familiar with those skilled in the art in the technical scope that the present invention discloses; the change that can expect easily or replacement, all should be encompassed within protection scope of the present invention.
Claims (9)
1. a nanometer particle-modified binding agent, comprises binding agent main body and Nano filling, it is characterized in that, described binding agent main body comprises: silicone resin 45-55wt.%, glass powder 25-35wt.% and boron carbide powder 15-20wt.%; Described Nano filling comprises: to account for the part by weight of described binding agent main body, nanometer aluminium powder 5-10wt.%, nano silica fume 5-10wt.% and alumina whisker 1-2wt.%.
2. nanometer particle-modified binding agent according to claim 1, is characterized in that,
Described glass powder, granularity is 400 ~ 500 orders, and fusing point is 400 ~ 500 DEG C;
Described boron carbide powder, granularity is 225 ~ 300 orders.
3. a preparation method for nanometer particle-modified binding agent as claimed in claim 1, comprises the preparation of binding agent main body, Nano filling preparation and the nano modification of binding agent, it is characterized in that,
(1) binding agent main body preparation: take a certain amount of binding agent host component by the dosage principle of binding agent host component, described silicone resin is put into wide neck flask, and add the organic solvent with described silicone resin equivalent, heating in water bath, stirring, until described silicone resin all dissolves, wherein, during described heating in water bath, constantly in wide neck flask, instill described organic solvent, be as the criterion just to keep solution mobility in wide-necked bottle; Then described glass powder and described boron carbide powder are added in described wide neck flask and stir 1 ~ 3 hour, constantly the described organic solvent of instillation, makes all substances in described wide neck flask mix completely, and ensures mobility, be then placed in ventilation and store for future use;
(2) Nano filling preparation: take a certain amount of nanofiller component by the dosage principle of nanofiller component, described nanometer aluminium powder and nano silica fume are put into deionized water makes it mix, form mixing solutions, add account for described mixing solutions weight 0.5wt.% Sodium hexametaphosphate 99 as dispersion agent, stirring at normal temperature 1 hour, sonic oscillation post-drying are for subsequent use; Described alumina whisker is put into deionized water, and adds coupling agent solution, sonic oscillation post-drying is for subsequent use;
(3) nano modification of binding agent: Nano filling prepared by described step (2) is joined in the binding agent main body of described step (1), heating in water bath, stirring and the described organic solvent of continuous instillation, after 1 ~ 3 hour, stop adding solvent, continuation heating in water bath and stirring are until solution becomes sticky thick, by the state that glass stick can just be provoked, described binding agent is ready to complete.
4. the preparation method of nanometer particle-modified binding agent according to claim 3, it is characterized in that, described coupling agent solution is: coupling agent adds in ethanol-water solution, accounting for ethanol-water solution weight percent according to coupling agent is that the proportioning of 0.2wt.% ~ 1wt.% mixes, and regulates pH to be 5.5 ~ 6.5; In wherein said ethanol-water solution, ethanol and water ratio are 1:1 ~ 2:1, and described coupling agent is silane coupling agent KH-540.
5. the preparation method of nanometer particle-modified binding agent according to claim 3, is characterized in that, described in described step (1) and described step (3), organic solvent is dimethylbenzene.
6. the preparation method of nanometer particle-modified binding agent according to claim 3, it is characterized in that, step (1) and step (3) water bath heating temperature are 60 DEG C, and described step (2) described sonic oscillation is 30min, and described bake out temperature is 80 DEG C.
7. a using method for nanometer particle-modified binding agent as claimed in claim 1, is characterized in that, comprises the step that object bonding, thermal treatment and CVI deposit:
(1) object bonding: sand paper polishes evenly cutting after to be bonded of object, and described groove depth is 0.5mm, and in alcohol sonic oscillation post-drying, then be applied on to be bonded by even for described binding agent, the docking of to be bonded of two articles, bubble is got rid of in the left and right changing of the relative positions simultaneously, fixes with fixture;
(2) thermal treatment: object after bonding is put into process furnace, with ramp to the 200 DEG C insulation 2 hours of 5 DEG C/min ~ 10 DEG C/min under protective atmosphere, then with ramp to the 1000 DEG C insulation 2 hours of 5 DEG C/min ~ 10 DEG C/min;
(3) CVI deposition: the described object after thermal treatment puts into chemical vapor deposition stove, passes into methane-propane mixture body, and control temperature is 1000 ~ 1500 DEG C, and pressure range is 2K ~ 5KPa, carries out vapour deposition.
8. the using method of nanometer particle-modified binding agent according to claim 7, is characterized in that, the described protective atmosphere in step (2) is argon gas, and flow is 50ml/min ~ 100ml/min.
9. the using method of nanometer particle-modified binding agent according to claim 7, is characterized in that, in described methane-propane mixture body, methane and propane volume ratio are 1:1 ~ 3:1.
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| CN105696408A (en) * | 2016-04-05 | 2016-06-22 | 哈尔滨理工大学 | Nano modified paper based on surface modification and preparation method thereof |
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| CN108611047A (en) * | 2018-05-30 | 2018-10-02 | 中国民航大学 | A method of preparing the wide organopolysiloxane base adhesive in temperature in use domain |
| CN108794042A (en) * | 2018-07-13 | 2018-11-13 | 航天材料及工艺研究所 | A kind of binder for porous ceramics and preparation method thereof and application method |
| CN108822792A (en) * | 2018-07-13 | 2018-11-16 | 中国民航大学 | A kind of high temperature adhesive preparation method suitable for nickel-base alloy |
| CN108794042B (en) * | 2018-07-13 | 2020-11-10 | 航天材料及工艺研究所 | Binder for porous ceramic and preparation method and use method thereof |
| WO2020224093A1 (en) * | 2019-05-06 | 2020-11-12 | 深圳市华星光电技术有限公司 | Composition material for peeling of flexible substrate, preparation method therefor, and fabrication method of flexible panel |
| CN111452458A (en) * | 2020-05-07 | 2020-07-28 | 上海均达科技发展有限公司 | Organic silicon few-glue polyimide film glass powder mica tape |
| CN113666755A (en) * | 2021-07-14 | 2021-11-19 | 山东格瑞兰德添加剂有限公司 | Organic ceramic firing binder and preparation method thereof |
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