CN100537807C - ZnO coating aluminum boric acid crystal whisker reinforcing aluminum base composite material and preparation method thereof - Google Patents

ZnO coating aluminum boric acid crystal whisker reinforcing aluminum base composite material and preparation method thereof Download PDF

Info

Publication number
CN100537807C
CN100537807C CNB2007101448551A CN200710144855A CN100537807C CN 100537807 C CN100537807 C CN 100537807C CN B2007101448551 A CNB2007101448551 A CN B2007101448551A CN 200710144855 A CN200710144855 A CN 200710144855A CN 100537807 C CN100537807 C CN 100537807C
Authority
CN
China
Prior art keywords
aluminum
composite material
boric acid
zno
base composite
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.)
Expired - Fee Related
Application number
CNB2007101448551A
Other languages
Chinese (zh)
Other versions
CN101195885A (en
Inventor
关丽娜
耿林
郑镇洙
吕奎明
李爱滨
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 Institute of Technology
Original Assignee
Harbin Institute of Technology
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 Institute of Technology filed Critical Harbin Institute of Technology
Priority to CNB2007101448551A priority Critical patent/CN100537807C/en
Publication of CN101195885A publication Critical patent/CN101195885A/en
Application granted granted Critical
Publication of CN100537807C publication Critical patent/CN100537807C/en
Expired - Fee Related legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Landscapes

  • Manufacture Of Alloys Or Alloy Compounds (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

ZnO coating aluminum boric acid crystal whisker reinforcing aluminum base composite material and preparation method thereof, it relates to a kind of matrix material and preparation method thereof.Its solves existing matrix material mesoboric acid aluminium whiskers and the matrix wettability is poor, with matrix in element generation surface reaction and prepare aluminum borate reinforced aluminum matrix composites complex process, cost height and the uneven problem of material structure.Its method is a preparation ZnO coated aluminium borate whister, molten alloy again, in the alloy under the semi-solid state, add the good ZnO coated aluminium borate whister of preheating then, carry out the semi-solid state mechanical stirring and get semi solid slurry, get the ZnO coating aluminum boric acid crystal whisker reinforcing aluminum base composite material through the semi-solid state extrusion molding.The present invention has increased aluminium borate whisker and matrix wettability, has stoped element generation surface reaction in the matrix, and the technology of preparation aluminum borate reinforced aluminum matrix composites is simple, cost is low and material structure is even.

Description

ZnO coating aluminum boric acid crystal whisker reinforcing aluminum base composite material and preparation method thereof
Technical field
The present invention relates to a kind of matrix material and preparation method thereof.
Background technology
At present, the main preparation technology of aluminum borate reinforced aluminum matrix composites is two kinds of powder metallurgy and extrusion castings.In the powder metallurgical technique; the whisker that some length are bigger is not easy homogenizing when mixing with metal-powder, simultaneously, and for not destroying whisker; abundant ball milling; in fact the microsegregation of whisker in matrix is more serious, must give by follow-up extrusion process perfect, in addition; because equipment and complex process; and cold and hot pressure must carry out under vacuum or protective atmosphere, so the cost height of powder metallurgic method is restricted its application.The temperature of reaction height of Extrution casting technique, response intensity is violent, and the preparation of prefabricated component also is difficult to control, and this kind method is because complex process, and the cost height is not suitable for scale operation.Adopt existing prepared aluminum boric acid crystal whisker reinforcing aluminum base composite material, aluminium borate whisker and matrix alloy react and generate brittle magnesium-aluminium spinel, destroy the integrity of whisker, influence the performance of material, and the wettability between whisker and the matrix is very poor, and be difficult to make the low matrix material of whisker volume fraction, and whisker accounts for 20~40% of total composite volume, and material structure is inhomogeneous.
Summary of the invention
The present invention seeks to for solve existing matrix material mesoboric acid aluminium whiskers and the matrix wettability is poor, with matrix in element generation surface reaction and prepare aluminum borate reinforced aluminum matrix composites complex process, cost height and the uneven problem of material structure, and provide a kind of ZnO coating aluminum boric acid crystal whisker reinforcing aluminum base composite material and preparation method thereof.
ZnO coating aluminum boric acid crystal whisker reinforcing aluminum base composite material of the present invention is synthetic by ZnO coated aluminium borate whister and alloy matrix aluminum processing, and wherein the ZnO coated aluminium borate whister accounts for 1~15% of total composite volume.
The preparation method of ZnO coating aluminum boric acid crystal whisker reinforcing aluminum base composite material realizes according to the following steps: one, be that the aluminium borate whisker of 100g/L and concentration are 70% hydrofluoric acid by 1: 480~520 mixed in molar ratio with concentration, leaving standstill and making the pH value with distilled water washing and precipitating thing behind 5~7h is 6~8, oven dry then gets purified aluminium borate whisker; Two, in proportion 1 mole of purified aluminium borate whisker, 27600~28000 moles of distilled water and 45~55 moles of zinc chloride are mixed stirring, ultra-sonic dispersion 30~60min after-filtration, oven dry, put into process furnace then, be warmed up to 480~520 ℃ and calcine 1~3h with the speed of 20 ℃/min, furnace cooling takes out then; Three, add distilled water in calcining in the after product, stir and ultra-sonic dispersion 25~35min after dry, through grinding disperse the ZnO coated aluminium borate whister, and preheating under 450~550 ℃ condition; Four, with the alloy matrix aluminum melting, being cooled to the semi-solid temperature interval again and controlling fraction solid is 35%~75%, adds the ZnO coated aluminium borate whister of preheating then, carries out the semi-solid state mechanical stirring in ar gas environment, gets semi solid slurry; Five, semi solid slurry being poured into preheating temperature is in 430~470 ℃ the mould, under the pressure of 180~220MPa with the speed that the presses down compacting of 15mm/s, pressurize 3~5min again; Six, compacting disposed slurry and mould are incubated 15~25min under 420~460 ℃ condition, then under the pressure of 180~220MPa with the extrusion speed extrusion bar of 15mm/s, the ZnO coating aluminum boric acid crystal whisker reinforcing aluminum base composite material.
The reaction of zinc chloride and aluminum borate forms ZnO and is coated on the aluminium borate whisker surface among the present invention, strengthened the wettability of aluminium borate whisker and matrix, improved the interface of aluminium borate whisker and matrix, ZnO can effectively stop the reaction of element in aluminium borate whisker and the matrix, and performance significantly improves; Adopt the churned mechanically method of semi-solid state to prepare semi solid slurry, directly extrusion molding prepares the ZnO coating aluminum boric acid crystal whisker reinforcing aluminum base composite material, realizes the short flow preparation of matrix material, and experimental installation is simple, saves the energy, can be used for scale operation.The present invention has improved that aluminium borate whisker is floating, segregation, non-wetted problem; Processing temperature is low, resistance to deformation is low, accomplishes less or does not have a machining, save energy; But once-forming has reduced operation, boosts productivity; Semi-solid-state shaping spare homogeneous microstructure, tiny, fine and close, product performance are high; Applied range, all aluminium alloys with solid-liquid two-phase region all can be used; Prepare the ZnO coated aluminium borate whister and account for 1~15% aluminum boric acid crystal whisker reinforcing aluminum base composite material of total composite volume, material structure is even.
Description of drawings
Fig. 1 is the stereoscan photograph of preparation gained ZnO coated aluminium borate whister in the embodiment three, Fig. 2 be in the embodiment 12 not the aluminium borate whisker of clading ZnO strengthen the stereoscan photograph of 6061 aluminum matrix composites, Fig. 3 is the stereoscan photograph that gained ZnO coated aluminium borate whister strengthens 6061 aluminum matrix composites in the embodiment 12.
Embodiment
Embodiment one: present embodiment ZnO coating aluminum boric acid crystal whisker reinforcing aluminum base composite material is synthetic by ZnO coated aluminium borate whister and alloy matrix aluminum processing, and wherein the ZnO coated aluminium borate whister accounts for 1~15% of total composite volume.
Embodiment two: the ZnO coated aluminium borate whister that is not both of present embodiment and embodiment one accounts for 8% of total composite volume.Other is identical with embodiment one.
Embodiment three: the method for preparing the ZnO coating aluminum boric acid crystal whisker reinforcing aluminum base composite material realizes according to the following steps: one, be that the aluminium borate whisker of 100g/L and concentration are 70% hydrofluoric acid by 1: 480~520 mixed in molar ratio with concentration, leaving standstill and making the pH value with distilled water washing and precipitating thing behind 5~7h is 6~8, oven dry then gets purified aluminium borate whisker; Two, in proportion 1 mole of purified aluminium borate whisker, 27600~28000 moles of distilled water and 45~55 moles of zinc chloride are mixed stirring, ultra-sonic dispersion 30~60min after-filtration, oven dry, put into process furnace then, be warmed up to 480~520 ℃ and calcine 1~3h with the speed of 20 ℃/min, furnace cooling takes out then; Three, add distilled water in calcining in the after product, stir and ultra-sonic dispersion 25~35min after dry, through grinding disperse the ZnO coated aluminium borate whister, and preheating under 450~550 ℃ condition; Four, with the alloy matrix aluminum melting, being cooled to the semi-solid temperature interval again and controlling fraction solid is 35%~75%, adds the ZnO coated aluminium borate whister of preheating then, carries out the semi-solid state mechanical stirring in ar gas environment, gets semi solid slurry; Five, semi solid slurry being poured into preheating temperature is in 430~470 ℃ the mould, under the pressure of 180~220MPa with the speed that the presses down compacting of 15mm/s, pressurize 3~5min again; Six, compacting disposed slurry and mould are incubated 15~25min under 420~460 ℃ condition, then under the pressure of 180~220MPa with the extrusion speed extrusion bar of 15mm/s, the ZnO coating aluminum boric acid crystal whisker reinforcing aluminum base composite material.
In the present embodiment step 2 purified aluminium borate whisker, distilled water and zinc chloride being mixed, is to add purified aluminium borate whisker earlier, and ultra-sonic dispersion 30min slowly adds zinc chloride again, adds ammoniacal liquor adjusting pH value then and reaches 7~9, again ultra-sonic dispersion 30min.
Embodiment four: not being both in the step 1 of present embodiment and embodiment three is that the aluminium borate whisker of 100g/L and concentration are 70% hydrofluoric acid by 1: 500 mixed in molar ratio with concentration.Other step and parameter are identical with embodiment three.
Embodiment five: not being both of present embodiment and embodiment three left standstill in the step 1 and made the pH value with distilled water washing and precipitating thing behind the 6h is 7.Other step and parameter are identical with embodiment three.
Embodiment six: present embodiment is mixed stirring, ultra-sonic dispersion 45min with 1 mole of purified aluminium borate whisker, 27800 moles of distilled water and 50 moles of zinc chloride in proportion with not being both in the step 2 of embodiment three.Other step and parameter are identical with embodiment three.
Embodiment seven: not being both of present embodiment and embodiment three is warmed up to 500 ℃ and calcine 2h in the step 2.Other step and parameter are identical with embodiment three.
Embodiment eight: the different of present embodiment and embodiment three are to dry behind the ultra-sonic dispersion 30min in the step 3, through grinding disperse the ZnO coated aluminium borate whister, and preheating under 500 ℃ condition.Other step and parameter are identical with embodiment three.
Embodiment nine: not being both in the step 4 the alloy matrix aluminum melting of present embodiment and embodiment three, it is interval and to control fraction solid be 50% to be cooled to semi-solid temperature again.Other step and parameter are identical with embodiment three.
Embodiment ten: it is in 450 ℃ the mould that not being both in the step 5 of present embodiment and embodiment three is poured into semi solid slurry preheating temperature, under the pressure of 200MPa with the speed that the presses down compacting of 15mm/s, pressurize 4min again.Other step and parameter are identical with embodiment three.
Embodiment 11: not being both in the step 6 of present embodiment and embodiment three is incubated 20min with compacting disposed slurry and mould under 440 ℃ condition, then under the pressure of 200MPa with the extrusion speed extrusion bar of 15mm/s.Other step and parameter are identical with embodiment three.
Embodiment 12: the method that present embodiment prepares the ZnO coating aluminum boric acid crystal whisker reinforcing aluminum base composite material realizes according to the following steps: aluminium borate whisker and the concentration that one, is 100g/L with concentration be after 70% hydrofluoric acid mixed in 1: 500 in molar ratio throw out, leave standstill behind the 6h to clean to the pH value and reach 7 with distilled water, oven dry then gets purified aluminium borate whisker; Two, in proportion 1 mole of purified aluminium borate whisker, 27800 moles of distilled water and 50 moles of zinc chloride are mixed stirring, ultra-sonic dispersion 45min after-filtration, oven dry, put into process furnace then, be warmed up to 500 ℃ and calcine 2h with the speed of 20 ℃/min, furnace cooling takes out then; Three, add distilled water in calcining in the after product, stir and ultra-sonic dispersion 30min after dry, through grinding disperse the ZnO coated aluminium borate whister, preheating under 500 ℃ condition; Four, with 6061 alloy matrix aluminum meltings, being cooled to 585 ℃~652 ℃ semi-solid temperature interval again and controlling fraction solid is 50%, the ZnO coated aluminium borate whister that adds preheating then, in ar gas environment, stirring intensity with 610 ℃ whipping temps, 300r/min carries out the semi-solid state mechanical stirring, gets semi solid slurry; Five, semi solid slurry being poured into preheating temperature is in 450 ℃ the mould, under the pressure of 200MPa with the speed that the presses down compacting of 15mm/s, pressurize 4min; Six, compacting disposed slurry and mould are incubated 20min under 440 ℃ condition, then under the pressure of 200MPa with the extrusion speed extrusion bar of 15mm/s, get the ZnO coated aluminium borate whister and strengthen 6061 aluminum matrix composites, wherein the ZnO coated aluminium borate whister accounts for 5% of total composite volume.
Present embodiment gained ZnO coated aluminium borate whister strengthens 6061 aluminum matrix composites and strengthens 6061 aluminum matrix composites with the aluminium borate whisker of not clading ZnO of preparation under the same conditions and compare, shown in Fig. 2 and 3, can find out among Fig. 2 that the aluminium borate whisker of clading ZnO does not strengthen 6061 aluminum matrix composites only stirs into a spot of whisker in the semi-solid state stirring technique, wettability between aluminium borate whisker and the matrix is very poor, and serious surface reaction takes place in element in whisker and the matrix, whisker is by havoc, but the surface reaction between ZnO coated aluminium borate whister and the matrix is prevented from substantially as can be seen from Figure 3, increased the wettability between whisker and the matrix, and the amount of stirring into of whisker obviously increases, and material structure is even.

Claims (10)

1, ZnO coating aluminum boric acid crystal whisker reinforcing aluminum base composite material, it is characterized in that the ZnO coating aluminum boric acid crystal whisker reinforcing aluminum base composite material is synthetic by ZnO coated aluminium borate whister and alloy matrix aluminum processing, wherein the ZnO coated aluminium borate whister accounts for 1~15% of total composite volume.
2, the method for preparing the described ZnO coating aluminum boric acid crystal whisker reinforcing aluminum base composite material of claim 1, it is characterized in that this method realizes according to the following steps: one, be that the aluminium borate whisker of 100g/L and concentration are 70% hydrofluoric acid by 1: 480~520 mixed in molar ratio with concentration, leaving standstill and making the pH value with distilled water washing and precipitating thing behind 5~7h is 6~8, oven dry then gets purified aluminium borate whisker; Two, in proportion 1 mole of purified aluminium borate whisker, 27600~28000 moles of distilled water and 45~55 moles of zinc chloride are mixed stirring, ultra-sonic dispersion 30~60min after-filtration, oven dry, put into process furnace then, be warmed up to 480~520 ℃ and calcine 1~3h with the speed of 20 ℃/min, furnace cooling takes out then; Three, add distilled water in calcining in the after product, stir and ultra-sonic dispersion 25~35min after dry, through grinding disperse the ZnO coated aluminium borate whister, and preheating under 450~550 ℃ condition; Four, with the alloy matrix aluminum melting, being cooled to the semi-solid temperature interval again and controlling fraction solid is 35%~75%, adds the ZnO coated aluminium borate whister of preheating then, carries out the semi-solid state mechanical stirring in ar gas environment, gets semi solid slurry; Five, semi solid slurry being poured into preheating temperature is in 430~470 ℃ the mould, under the pressure of 180~220MPa with the speed that the presses down compacting of 15mm/s, pressurize 3~5min again; Six, compacting disposed slurry and mould are incubated 15~25min under 420~460 ℃ condition, then under the pressure of 180~220MPa with the extrusion speed extrusion bar of 15mm/s, the ZnO coating aluminum boric acid crystal whisker reinforcing aluminum base composite material.
3, the method for preparing the ZnO coating aluminum boric acid crystal whisker reinforcing aluminum base composite material according to claim 2 is characterized in that in the step 1 with concentration being that aluminium borate whisker and the concentration of 100g/L is that 70% hydrofluoric acid mixed in 1: 500 in molar ratio.
4, the method for preparing the ZnO coating aluminum boric acid crystal whisker reinforcing aluminum base composite material according to claim 2 is characterized in that leaving standstill in the step 1 behind the 6h cleaning to the pH value with distilled water and reaches 7.
5, the method for preparing the ZnO coating aluminum boric acid crystal whisker reinforcing aluminum base composite material according to claim 2, it is characterized in that in proportion 1 mole of purified aluminium borate whisker, 27800 moles of distilled water and 50 moles of zinc chloride being mixed in the step 2 and stir ultra-sonic dispersion 45min.
6, the method for preparing the ZnO coating aluminum boric acid crystal whisker reinforcing aluminum base composite material according to claim 2 is characterized in that being warmed up in the step 2 500 ℃ and calcine 2h.
7, the method for preparing the ZnO coating aluminum boric acid crystal whisker reinforcing aluminum base composite material according to claim 2 is characterized in that drying behind the ultra-sonic dispersion 30min in the step 3, through grinding disperse the ZnO coated aluminium borate whister, and preheating under 500 ℃ condition.
8, the method for preparing the ZnO coating aluminum boric acid crystal whisker reinforcing aluminum base composite material according to claim 2 is characterized in that the control fraction solid is 50% in the step 4.
9, the method for preparing the ZnO coating aluminum boric acid crystal whisker reinforcing aluminum base composite material according to claim 2, it is characterized in that in the step 5 semi solid slurry is poured into preheating temperature and be in 450 ℃ the mould, under the pressure of 200MPa with the speed that the presses down compacting of 15mm/s, pressurize 4min.
10, the method for preparing the ZnO coating aluminum boric acid crystal whisker reinforcing aluminum base composite material according to claim 2, it is characterized in that in the step 6 compacting disposed slurry and mould being incubated 20min under 440 ℃ condition, then under the pressure of 200MPa with the extrusion speed extrusion bar of 15mm/s.
CNB2007101448551A 2007-12-19 2007-12-19 ZnO coating aluminum boric acid crystal whisker reinforcing aluminum base composite material and preparation method thereof Expired - Fee Related CN100537807C (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CNB2007101448551A CN100537807C (en) 2007-12-19 2007-12-19 ZnO coating aluminum boric acid crystal whisker reinforcing aluminum base composite material and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CNB2007101448551A CN100537807C (en) 2007-12-19 2007-12-19 ZnO coating aluminum boric acid crystal whisker reinforcing aluminum base composite material and preparation method thereof

Publications (2)

Publication Number Publication Date
CN101195885A CN101195885A (en) 2008-06-11
CN100537807C true CN100537807C (en) 2009-09-09

Family

ID=39546511

Family Applications (1)

Application Number Title Priority Date Filing Date
CNB2007101448551A Expired - Fee Related CN100537807C (en) 2007-12-19 2007-12-19 ZnO coating aluminum boric acid crystal whisker reinforcing aluminum base composite material and preparation method thereof

Country Status (1)

Country Link
CN (1) CN100537807C (en)

Families Citing this family (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102071373B (en) * 2011-02-14 2012-06-27 哈尔滨理工大学 Method for preparing Cr2O3 coated aluminum borate whisker reinforced aluminum matrix composites
CN102168232B (en) * 2011-03-30 2012-07-04 哈尔滨理工大学 Preparation method of aluminum based composite material reinforced by aluminium borate whisker coated with CuO
CN102433520B (en) * 2011-12-21 2013-04-10 哈尔滨工业大学 ZnWO4-coated aluminum borate whisker-reinforced aluminum matrix composite and preparation method thereof
CN106282855A (en) * 2016-09-28 2017-01-04 广州凯耀资产管理有限公司 A kind of inorganic crystal whisker strengthens magnesium base composite material and preparation method thereof
CN109207781A (en) * 2018-09-17 2019-01-15 南昌大学 A kind of pressing method improving 7075 aluminium alloys
CN110863160A (en) * 2019-11-11 2020-03-06 中国科学院上海硅酸盐研究所 SIALON whisker reinforced aluminum matrix composite material and preparation method thereof
CN112648104B (en) * 2020-12-07 2022-07-19 中国兵器科学研究院宁波分院 Whisker reinforced aluminum alloy piston and preparation method thereof

Also Published As

Publication number Publication date
CN101195885A (en) 2008-06-11

Similar Documents

Publication Publication Date Title
CN100537807C (en) ZnO coating aluminum boric acid crystal whisker reinforcing aluminum base composite material and preparation method thereof
CN105200272B (en) A kind of extrusion casting method of wrought aluminium alloy lampshade
CN103320651B (en) Fine-grained zinc-based alloy for die and preparation process thereof
CN107893170A (en) A kind of vehicle body in-situ nano reinforced aluminium alloy squeeze wood and preparation method
CN101787472B (en) Heat-resistant forged magnesium-rare earth alloy and preparation method thereof
CN110423915B (en) Preparation method of aluminum-based composite material
CN115505795A (en) Heat-treatment-free aluminum alloy material and forming process thereof
CN110423914B (en) Preparation method of rare earth magnesium alloy composite material
CN110423935B (en) Light metal composite material taking rare earth oxide as reinforcement
CN101565782B (en) Method for adding carbon nano tube into metal bath
CN110438379B (en) Preparation method of lithium-containing magnesium/aluminum-based composite material
CN105385917A (en) High-strength high-plasticity magnesium alloy and preparation method thereof
CN103170600A (en) Aluminum-silicon alloy brake-separating piece semisolid rheological diecasting forming process
CN106755724B (en) A kind of smelting technology being suitable for 3 tons of intermediate frequency furnace production nodulizers
CN106676345A (en) Super-strength aluminum alloy section
CN110317970A (en) A kind of Cu-Cr-Zr alloy, preparation method and applications
CN109943742A (en) A kind of alloy improved materials and preparation method thereof
CN109988952A (en) A kind of preparation method of aluminum alloy mobile phone shell
CN114833329A (en) High-entropy alloy multi-section mixed casting device and method thereof
CN114438373A (en) Bright anodized extrusion casting aluminum alloy and preparation method thereof
CN103695673B (en) A kind of intermetallic compound particle Al 3the preparation method of-M reinforced aluminum matrix composites
WO2021035776A1 (en) Method for preparing magnesium-based composite material
CN209407363U (en) A kind of high-efficiency insulated device of aluminum products production
CN110408848A (en) Anti-corrosion mold cast slab and its process
CN110343895A (en) TiB in situ2The preparation method of particle REINFORCED Al Cu based composites

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant
C17 Cessation of patent right
CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20090909

Termination date: 20111219