CN105177538A - Preparation method for nano-copper coated single crystal sapphire fiber - Google Patents
Preparation method for nano-copper coated single crystal sapphire fiber Download PDFInfo
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- CN105177538A CN105177538A CN201510588770.7A CN201510588770A CN105177538A CN 105177538 A CN105177538 A CN 105177538A CN 201510588770 A CN201510588770 A CN 201510588770A CN 105177538 A CN105177538 A CN 105177538A
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- monocrystalline sapphire
- coated
- copper
- sapphire whisker
- whisker
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- 229910052594 sapphire Inorganic materials 0.000 title claims abstract description 133
- 239000010980 sapphire Substances 0.000 title claims abstract description 133
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 76
- 239000010949 copper Substances 0.000 title claims abstract description 76
- 239000000835 fiber Substances 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000013078 crystal Substances 0.000 title abstract description 15
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 70
- 239000000243 solution Substances 0.000 claims abstract description 39
- 239000011259 mixed solution Substances 0.000 claims abstract description 36
- 229910000033 sodium borohydride Inorganic materials 0.000 claims abstract description 26
- 239000012279 sodium borohydride Substances 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 19
- 238000005406 washing Methods 0.000 claims abstract description 14
- 230000009467 reduction Effects 0.000 claims abstract description 9
- 230000008569 process Effects 0.000 claims abstract description 8
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 40
- 238000003756 stirring Methods 0.000 claims description 21
- 229910021529 ammonia Inorganic materials 0.000 claims description 20
- 238000001035 drying Methods 0.000 claims description 18
- -1 copper complex ion Chemical class 0.000 claims description 16
- 238000001556 precipitation Methods 0.000 claims description 14
- 238000013019 agitation Methods 0.000 claims description 9
- 238000009736 wetting Methods 0.000 claims description 9
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 7
- 230000004048 modification Effects 0.000 claims description 7
- 238000012986 modification Methods 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 claims description 6
- 239000002905 metal composite material Substances 0.000 claims description 5
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims description 4
- FGUUSXIOTUKUDN-IBGZPJMESA-N C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 Chemical compound C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 FGUUSXIOTUKUDN-IBGZPJMESA-N 0.000 claims description 2
- 150000001879 copper Chemical class 0.000 claims description 2
- 229910000365 copper sulfate Inorganic materials 0.000 claims description 2
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 2
- NWFNSTOSIVLCJA-UHFFFAOYSA-L copper;diacetate;hydrate Chemical compound O.[Cu+2].CC([O-])=O.CC([O-])=O NWFNSTOSIVLCJA-UHFFFAOYSA-L 0.000 claims description 2
- 229960003280 cupric chloride Drugs 0.000 claims description 2
- 239000012266 salt solution Substances 0.000 claims description 2
- 238000005516 engineering process Methods 0.000 abstract description 2
- 238000001914 filtration Methods 0.000 abstract 1
- 150000002500 ions Chemical class 0.000 abstract 1
- 239000002131 composite material Substances 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 5
- 235000011149 sulphuric acid Nutrition 0.000 description 5
- 239000001117 sulphuric acid Substances 0.000 description 5
- 239000011159 matrix material Substances 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000011157 advanced composite material Substances 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- OJMOMXZKOWKUTA-UHFFFAOYSA-N aluminum;borate Chemical compound [Al+3].[O-]B([O-])[O-] OJMOMXZKOWKUTA-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 229910001092 metal group alloy Inorganic materials 0.000 description 1
- 239000011156 metal matrix composite Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Landscapes
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention provides a preparation method for a nano-copper coated single crystal sapphire fiber. The method includes the steps that a, an alkaline sodium borohydride reduction solution is prepared at a room temperature; b, a reduction mixed solution for single crystal sapphire whiskers is prepared; c, a dark blue solution containing complex copper ammine ions is prepared; d, the mixed solution prepared in the step b and the mixed solution prepared in the step c are mixed so that a nano-copper coated single crystal sapphire mixed solution can be prepared; e, filtering and washing are performed so that wet nano-copper coated single crystal sapphire whiskers can be obtained; and f, the wet nano-copper coated single crystal sapphire whiskers are dried so that single crystal sapphire whiskers with the surfaces coated with nano-copper can be obtained. According to the method for the copper-coated modified single crystal sapphire whiskers, operation in the experimental process is easy, industrialization can be easily achieved through the technology, and good application prospects are achieved.
Description
Technical field
The invention belongs to field of compound material, particularly the preparation method of the coated monocrystalline sapphire fiber of a kind of Nanometer Copper.
Background technology
Monocrystalline sapphire fiber is a kind of signle crystal alumina fiber (whisker) with certain length-to-diameter ratio, and it is completely different with preparation method from semiconducter substrate sapphire wafer material applications.High-melting-point, high strength, high-modulus, to be able to bear strong corrosion be composite request to third generation advanced composite material.And monocrystalline sapphire fiber is the optimal selection meeting composite request at present.
Metal-base composites be both there is metallic character by selecting optimum combination metallic matrix or alloy substrate and reinforce to obtain, there is again the material of high specific strength, high ratio modulus, heat-resisting, wear-resisting etc. over-all properties.Monocrystalline sapphire whisker (SinglecrystalsapphireWhisker) is the high purity single crystal of cultivating growth under controlled conditions, its crystalline structure is near-complete, not containing lattice defects such as boundary or grain, dislocation, cavities, have that proportion is little, the physicals of high strength, high-melting-point, high abrasion amount and high corrosion resistance, specific tenacity and the specific modulus of matrix material can be significantly improved.Monocrystalline sapphire whisker becomes the optimal selection of third generation advanced composite material.
After adding monocrystalline sapphire whisker in a metal, the bending elastic modulus of goods, tensile strength, dimensional stability and thermal distoftion temperature can be significantly improved.The component quality made with high specific strength, specific modulus matrix material is little, good rigidly, intensity are high, is the structured material of aerospace field middle ideal.Can be used as the surfacing of aircraft turbine engine and rocket engine hot-zone and supersonic plane.After inorganic crystal whisker adds metallic substance, the properties of metallic substance can be improved, aluminium borate whisker strengthens metal composite and to have succeeded application in metal alloy industry, resulting materials can be used on engine piston, connecting rod, on the heat-resistant parts such as compressor housing (wear quiet, Wang Min, Zhang Jincai. aluminium borate whisker application in the composite [J] chemical industry mineral and processing, 2005, (10): 36-38).The application of whisker in alloy filter, compressor blade and aviation etc. is also very extensive.
In metal-base composites, matrix accounts for very at high proportion, and generally more than 60%, good thermal conductivity can effectively be conducted heat, and reduce the gradient produced after component is heated, dispel the heat rapidly, this is particularly important to the component that dimensional stabilizing is high.Good electroconductibility can effectively prevent aircraft component from producing the problem of static focus simultaneously.
Due to the heat conduction of monocrystalline sapphire whisker, poorly conductive, bad with the wettability of metal, can not be formed firmly bonding with metal function, limit the application of monocrystalline sapphire whisker reinforced metal matrix composites.
Summary of the invention
The object of the present invention is to provide a kind of method utilizing coated copper modification monocrystalline sapphire whisker, the present invention effectively can improve wetting property when monocrystalline sapphire whisker and metal composite, solves the problem of electrical and thermal conductivity difference.
For realizing above object, technical scheme of the present invention is:
A preparation method for the coated monocrystalline sapphire fiber of Nanometer Copper, comprising: under a, room temperature, is joined by sodium borohydride in weak ammonia, stirs 1 ~ 5min, obtains alkaline sodium borohydride reduction solution; B, monocrystalline sapphire whisker is joined in above-mentioned alkaline sodium borohydride solution reduced liquid, with ultrasonic washing instrument to the solution ultrasonic disperse process containing monocrystalline sapphire whisker, obtain the reductibility mixed solution containing monocrystalline sapphire whisker; C, in copper salt solution, drip weak ammonia gradually, then have precipitation azury to generate, continue to drip ammoniacal liquor and dissolve completely to precipitation, now namely obtain the navy blue solution containing ammoniacal copper complex ion; D, magnetic agitation instrument is utilized to stir, in the reductibility mixed solution containing monocrystalline sapphire whisker, the solution containing ammoniacal copper complex ion is added with the speed of 5/min ~ 10 droplet/min, till monocrystalline sapphire whisker becomes redness, stop stirring, obtain the monocrystalline sapphire mixed solution that Nanometer Copper is coated; E, reacted monocrystalline sapphire mixed solution to be filtered, washing, the monocrystalline sapphire whisker that the Nanometer Copper obtaining wetting is coated; F, monocrystalline sapphire whisker coated for wet Nanometer Copper is carried out drying, surface can be obtained containing the coated monocrystalline sapphire whisker of Nanometer Copper.
In described step a, the mass ratio of sodium borohydride and weak ammonia is 1:1 ~ 50, and rare ammonia concn is 1 ~ 30% (w/v).
The temperature of ultrasonic washing instrument described in step b is 40 ~ 60 DEG C, and the treatment time is 5 ~ 10min.
In step b, the mass ratio of monocrystalline sapphire whisker and sodium borohydride is 1 ~ 1:10.
In step c, mantoquita is copper sulfate, cupric nitrate, cupric chloride, neutralized verdigris or their combination.
The concentration of described mantoquita is 1 ~ 30% (w/v), and rare ammonia concn is 1 ~ 30% (w/v), and the mass ratio of mantoquita used and monocrystalline sapphire whisker is 1 ~ 100:1.
In steps d, the rotating speed of magnetic agitation instrument is 250r/min ~ 500r/min, the speed adding the solution containing ammoniacal copper complex ion in the reductibility mixed solution containing monocrystalline sapphire whisker is 5/and min ~ 10 droplet/min.
After being filtered by reacted monocrystalline sapphire mixed solution in step e, the method for washing is: deionized water wash 2 ~ 5 times; Drying means in step f is: monocrystalline sapphire whisker coated for wet Nanometer Copper is carried out drying at temperature is 60 ~ 100 DEG C, and time of drying is 3 ~ 9h.
A kind of metal composite, comprises the Nanometer Copper coating modification monocrystalline sapphire whisker that method of the present invention is obtained.
The invention has the beneficial effects as follows:
(1) the present invention aims to provide the method for the coated monocrystalline sapphire whisker of a kind of Nanometer Copper, the clad ratio on monocrystalline sapphire whisker surface 98% can be reached, monocrystalline sapphire whisker after copper clad not only keeps original premium properties, also have the wetting property good with metal composite, electroconductibility thermal conductivity is good.The copper clad modification monocrystalline sapphire whisker of gained can as the toughness reinforcing body of metal-base composites.
(2) method of copper clad modification monocrystalline sapphire whisker of the present invention, experimentation is simple to operate, and this technique easily realizes industrialization, has a good application prospect.
(3) method of copper clad modification monocrystalline sapphire whisker of the present invention, raw material is cheap, wide material sources, and has good environmental benefit and economic benefit.
Embodiment
The present invention is described in further detail by embodiment.
Embodiment 1
(1) under room temperature, 10g sodium borohydride being joined 20g concentration is in the weak ammonia of 1 ~ 30% (w/v), stirs 1 ~ 5min, obtains alkaline sodium borohydride reduction solution.
(2) 10g monocrystalline sapphire whisker is joined in above-mentioned alkaline sodium borohydride solution reduced liquid.In temperature be in the ultrasonic washing instrument of 40 ~ 60 DEG C to the solution ultrasonic disperse process 5 ~ 10min containing monocrystalline sapphire whisker, obtain the reductibility mixed solution containing monocrystalline sapphire whisker.
(3) in the sulphuric acid soln of 40g20%, drip weak ammonia gradually, then have precipitation azury to generate, continue to drip ammoniacal liquor and dissolve completely to precipitation, now namely obtain the navy blue solution containing ammoniacal copper complex ion.
(4) utilize magnetic agitation instrument under the stirring velocity of rotating speed for 250r/min ~ 500r/min, in the reductibility mixed solution containing monocrystalline sapphire whisker, the solution containing ammoniacal copper complex ion is added with the speed of 5/min ~ 10 droplet/min, till monocrystalline sapphire whisker becomes redness, stop stirring, obtain the monocrystalline sapphire mixed solution that Nanometer Copper is coated.
(5) reacted mixed solution is filtered, deionized water wash 2 ~ 3 times, the monocrystalline sapphire whisker that the Nanometer Copper obtaining wetting is coated.
(6) monocrystalline sapphire whisker coated for wet Nanometer Copper is carried out drying at temperature is 60 ~ 100 DEG C, time of drying is 3 ~ 9h, can obtain surface and contain the coated monocrystalline sapphire whisker of Nanometer Copper.Through measuring, productive rate reaches 85%, and the metallic copper of monocrystalline sapphire whisker surface containing 17.8% quality, monocrystalline sapphire whisker surface copper clad ratio is 88%.
Embodiment 2
(1) under room temperature, 20g sodium borohydride being joined 30g concentration is in the weak ammonia of 1 ~ 30% (w/v), stirs 1 ~ 5min, obtains alkaline sodium borohydride reduction solution.
(2) 10g monocrystalline sapphire whisker is joined in above-mentioned alkaline sodium borohydride solution reduced liquid.In temperature be in the ultrasonic washing instrument of 40 ~ 60 DEG C to the solution ultrasonic disperse process 5 ~ 10min containing monocrystalline sapphire whisker, obtain the reductibility mixed solution containing monocrystalline sapphire whisker.
(3) in the sulphuric acid soln of 40g10%, drip weak ammonia gradually, then have precipitation azury to generate, continue to drip ammoniacal liquor and dissolve completely to precipitation, now namely obtain the navy blue solution containing ammoniacal copper complex ion.
(4) utilize magnetic agitation instrument under the stirring velocity of rotating speed for 250r/min ~ 500r/min, in the reductibility mixed solution containing monocrystalline sapphire whisker, the solution containing ammoniacal copper complex ion is added with the speed of 5/min ~ 10 droplet/min, till monocrystalline sapphire whisker becomes redness, stop stirring, obtain the monocrystalline sapphire mixed solution that Nanometer Copper is coated.
(5) reacted mixed solution is filtered, deionized water wash 2 ~ 3 times, the monocrystalline sapphire whisker that the Nanometer Copper obtaining wetting is coated.
(6) monocrystalline sapphire whisker coated for wet Nanometer Copper is carried out drying at temperature is 60 ~ 100 DEG C, time of drying is 3 ~ 9h, can obtain surface and contain the coated monocrystalline sapphire whisker of Nanometer Copper.Through measuring, productive rate reaches 90%, and the metallic copper of monocrystalline sapphire whisker surface containing 19% quality, monocrystalline sapphire whisker surface copper clad ratio is 92%.
Embodiment 3
(1) under room temperature, 30g sodium borohydride being joined 50g concentration is in the weak ammonia of 1 ~ 30% (w/v), stirs 1 ~ 5min, obtains alkaline sodium borohydride reduction solution.
(2) 10g monocrystalline sapphire whisker is joined in above-mentioned alkaline sodium borohydride solution reduced liquid.In temperature be in the ultrasonic washing instrument of 40 ~ 60 DEG C to the solution ultrasonic disperse process 5 ~ 10min containing monocrystalline sapphire whisker, obtain the reductibility mixed solution containing monocrystalline sapphire whisker.
(3) in the sulphuric acid soln of 50g20%, drip weak ammonia gradually, then have precipitation azury to generate, continue to drip ammoniacal liquor and dissolve completely to precipitation, now namely obtain the navy blue solution containing ammoniacal copper complex ion.
(4) utilize magnetic agitation instrument under the stirring velocity of rotating speed for 250r/min ~ 500r/min, in the reductibility mixed solution containing monocrystalline sapphire whisker, the solution containing ammoniacal copper complex ion is added with the speed of 5/min ~ 10 droplet/min, till monocrystalline sapphire whisker becomes redness, stop stirring, obtain the monocrystalline sapphire mixed solution that Nanometer Copper is coated.
(5) reacted mixed solution is filtered, deionized water wash 2 ~ 3 times, the monocrystalline sapphire whisker that the Nanometer Copper obtaining wetting is coated.
(6) monocrystalline sapphire whisker coated for wet Nanometer Copper is carried out drying at temperature is 60 ~ 100 DEG C, time of drying is 3 ~ 9h, can obtain surface and contain the coated monocrystalline sapphire whisker of Nanometer Copper.Through measuring, productive rate reaches 90%, and the metallic copper of monocrystalline sapphire whisker surface containing 25% quality, monocrystalline sapphire whisker surface copper clad ratio is 94%.
Embodiment 4
(1) under room temperature, 40g sodium borohydride being joined 60g concentration is in the weak ammonia of 1 ~ 30% (w/v), stirs 1 ~ 5min, obtains alkaline sodium borohydride reduction solution.
(2) 10g monocrystalline sapphire whisker is joined in above-mentioned alkaline sodium borohydride solution reduced liquid.In temperature be in the ultrasonic washing instrument of 40 ~ 60 DEG C to the solution ultrasonic disperse process 5 ~ 10min containing monocrystalline sapphire whisker, obtain the reductibility mixed solution containing monocrystalline sapphire whisker.
(3) in the sulphuric acid soln of 50g30%, drip weak ammonia gradually, then have precipitation azury to generate, continue to drip ammoniacal liquor and dissolve completely to precipitation, now namely obtain the navy blue solution containing ammoniacal copper complex ion.
(4) utilize magnetic agitation instrument under the stirring velocity of rotating speed for 250r/min ~ 500r/min, in the reductibility mixed solution containing monocrystalline sapphire whisker, the solution containing ammoniacal copper complex ion is added with the speed of 5/min ~ 10 droplet/min, till monocrystalline sapphire whisker becomes redness, stop stirring, obtain the monocrystalline sapphire mixed solution that Nanometer Copper is coated.
(5) reacted mixed solution is filtered, deionized water wash 2 ~ 3 times, the monocrystalline sapphire whisker that the Nanometer Copper obtaining wetting is coated.
(6) monocrystalline sapphire whisker coated for wet Nanometer Copper is carried out drying at temperature is 60 ~ 100 DEG C, time of drying is 3 ~ 9h, can obtain surface and contain the coated monocrystalline sapphire whisker of Nanometer Copper.Through measuring, productive rate reaches 93%, and the metallic copper of monocrystalline sapphire whisker surface containing 28% quality, monocrystalline sapphire whisker surface copper clad ratio is 96%.
Embodiment 5
(1) under room temperature, 100g sodium borohydride being joined 80g concentration is in the weak ammonia of 1 ~ 30% (w/v), stirs 1 ~ 5min, obtains alkaline sodium borohydride reduction solution.
(2) 10g monocrystalline sapphire whisker is joined in above-mentioned alkaline sodium borohydride solution reduced liquid.In temperature be in the ultrasonic washing instrument of 40 ~ 60 DEG C to the solution ultrasonic disperse process 5 ~ 10min containing monocrystalline sapphire whisker, obtain the reductibility mixed solution containing monocrystalline sapphire whisker.
(3) in the sulphuric acid soln of 60g30%, drip weak ammonia gradually, then have precipitation azury to generate, continue to drip ammoniacal liquor and dissolve completely to precipitation, now namely obtain the navy blue solution containing ammoniacal copper complex ion.
(4) utilize magnetic agitation instrument under the stirring velocity of rotating speed for 250r/min ~ 500r/min, in the reductibility mixed solution containing monocrystalline sapphire whisker, the solution containing ammoniacal copper complex ion is added with the speed of 5/min ~ 10 droplet/min, till monocrystalline sapphire whisker becomes redness, stop stirring, obtain the monocrystalline sapphire mixed solution that Nanometer Copper is coated.
(5) reacted mixed solution is filtered, deionized water wash 2 ~ 3 times, the monocrystalline sapphire whisker that the Nanometer Copper obtaining wetting is coated.
(6) monocrystalline sapphire whisker coated for wet Nanometer Copper is carried out drying at temperature is 60 ~ 100 DEG C, time of drying is 3 ~ 9h, can obtain surface and contain the coated monocrystalline sapphire whisker of Nanometer Copper.Through measuring, productive rate reaches 95%, and the metallic copper of monocrystalline sapphire whisker surface containing 30% quality, monocrystalline sapphire whisker surface copper clad ratio is 98%.
Monocrystalline sapphire whisker embodiment 1 ~ 5 processed carries out the test of coating content, clad ratio, electroconductibility and thermal conductivity, characterize (the monocrystalline sapphire whisker that 0 representative does not have copper clad) coated monocrystalline sapphire whisker, its test result is as shown in table 1:
Table 1
Case study on implementation monocrystalline sapphire whisker surface copper content wt% monocrystalline sapphire whisker surface copper clad ratio copper clad monocrystalline sapphire crystal whisker conductive (s/m) copper clad monocrystalline sapphire crystal whisker conductive (w/mK)
| Case study on implementation | Monocrystalline sapphire whisker surface copper content wt% | Monocrystalline sapphire whisker surface copper clad ratio | Copper clad monocrystalline sapphire crystal whisker conductive (s/m) | Copper clad monocrystalline sapphire crystal whisker conductive (w/mK) |
| 0 | 0 | 0 | 1×10 -14 | 36 |
| 1 | 17.8% | 88 % | 2.42×10 6 | 115 |
| 2 | 19% | 92 % | 5.93×10 6 | 126 |
| 3 | 25% | 94% | 7.89×10 6 | 132 |
| 4 | 28% | 96% | 8.65×10 6 | 138 |
| 5 | 30% | 98% | 9.15×10 6 | 140 |
Note: in table, two parameters use power spectrum constituent content analysis method, x-ray photoelectron spectroscopy analytical method, current meter, thermal conductivity measuring apparatus respectively.
Above-described embodiment is only and technological thought of the present invention and feature is described, it describes comparatively concrete and detailed, its object is to enable those of ordinary skill in the art understand content of the present invention and implement according to this, therefore only the scope of the claims of the present invention can not be limited with this, it should be noted that, for the person of ordinary skill of the art, without departing from the inventive concept of the premise, some distortion and improvement can also be made, i.e. all any amendments done according to the embodiment of the present invention, equivalent variations and modification, all still belong in the scope of technical scheme of the present invention.
Claims (9)
1. a preparation method for the coated monocrystalline sapphire fiber of Nanometer Copper, comprising: under a, room temperature, is joined by sodium borohydride in weak ammonia, stirs 1 ~ 5min, obtains alkaline sodium borohydride reduction solution; B, monocrystalline sapphire whisker is joined in above-mentioned alkaline sodium borohydride solution reduced liquid, with ultrasonic washing instrument to the solution ultrasonic disperse process containing monocrystalline sapphire whisker, obtain the reductibility mixed solution containing monocrystalline sapphire whisker; C, in copper salt solution, drip weak ammonia gradually, then have precipitation azury to generate, continue to drip ammoniacal liquor and dissolve completely to precipitation, now namely obtain the navy blue solution containing ammoniacal copper complex ion; D, magnetic agitation instrument is utilized to stir, in the reductibility mixed solution containing monocrystalline sapphire whisker, at the uniform velocity add the solution containing ammoniacal copper complex ion, till monocrystalline sapphire whisker becomes redness, stop stirring, obtain the monocrystalline sapphire mixed solution that Nanometer Copper is coated; E, reacted monocrystalline sapphire mixed solution to be filtered, washing, the monocrystalline sapphire whisker that the Nanometer Copper obtaining wetting is coated; F, monocrystalline sapphire whisker coated for wet Nanometer Copper is carried out drying, surface can be obtained containing the coated monocrystalline sapphire whisker of Nanometer Copper.
2. the preparation method of the coated monocrystalline sapphire fiber of Nanometer Copper according to claim 1, in described step a, the mass ratio of sodium borohydride and weak ammonia is 1:1 ~ 50, and rare ammonia concn is 1 ~ 30% (w/v).
3. the preparation method of the coated monocrystalline sapphire fiber of Nanometer Copper according to claim 1, the temperature of ultrasonic washing instrument described in step b is 40 ~ 60 DEG C, and the treatment time is 5 ~ 10min.
4. the preparation method of the coated monocrystalline sapphire fiber of Nanometer Copper according to claim 1, in step b, the mass ratio of monocrystalline sapphire whisker and sodium borohydride is 1 ~ 1:10.
5. the preparation method of the coated monocrystalline sapphire fiber of Nanometer Copper according to claim 1, in step c, mantoquita is copper sulfate, cupric nitrate, cupric chloride, neutralized verdigris or their combination.
6. the preparation method of the coated monocrystalline sapphire fiber of Nanometer Copper according to claim 1, the concentration of described mantoquita is 1 ~ 30% (w/v), rare ammonia concn is 1 ~ 30% (w/v), and the mass ratio of mantoquita used and monocrystalline sapphire whisker is 1 ~ 100:1.
7. the preparation method of the coated monocrystalline sapphire fiber of Nanometer Copper according to claim 1, in steps d, the rotating speed of magnetic agitation instrument is 250r/min ~ 500r/min, the speed adding the solution containing ammoniacal copper complex ion in the reductibility mixed solution containing monocrystalline sapphire whisker is 5/and min ~ 10 droplet/min.
8. the preparation method of the coated monocrystalline sapphire fiber of Nanometer Copper according to claim 1, after being filtered by reacted monocrystalline sapphire mixed solution in step e, the method for washing is: deionized water wash 2 ~ 5 times; Drying means in step f is: monocrystalline sapphire whisker coated for wet Nanometer Copper is carried out drying at temperature is 60 ~ 100 DEG C, and time of drying is 3 ~ 9h.
9. a metal composite, comprises the copper clad modification monocrystalline sapphire whisker that the method described in any one of claim 1-8 obtains.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510588770.7A CN105177538B (en) | 2015-09-16 | 2015-09-16 | A kind of preparation method of nanometer of copper clad monocrystalline sapphire fiber |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510588770.7A CN105177538B (en) | 2015-09-16 | 2015-09-16 | A kind of preparation method of nanometer of copper clad monocrystalline sapphire fiber |
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| Publication Number | Publication Date |
|---|---|
| CN105177538A true CN105177538A (en) | 2015-12-23 |
| CN105177538B CN105177538B (en) | 2018-11-23 |
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| CN112530625A (en) * | 2020-11-05 | 2021-03-19 | 青岛大学 | Chitin whisker-based conductive material and preparation method thereof, and aqueous conductive ink and application thereof |
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| CN101517123A (en) * | 2006-09-15 | 2009-08-26 | 宇部日东化成株式会社 | Base material covered with metal layer and process for producing the same |
| CN102124142A (en) * | 2008-09-25 | 2011-07-13 | 宇部日东化成株式会社 | Method for forming metal coating film, and electrically conductive particle |
| CN103060779A (en) * | 2012-12-04 | 2013-04-24 | 复旦大学 | Preparation method of copper/modal fiber composite material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101517123A (en) * | 2006-09-15 | 2009-08-26 | 宇部日东化成株式会社 | Base material covered with metal layer and process for producing the same |
| CN102124142A (en) * | 2008-09-25 | 2011-07-13 | 宇部日东化成株式会社 | Method for forming metal coating film, and electrically conductive particle |
| CN103060779A (en) * | 2012-12-04 | 2013-04-24 | 复旦大学 | Preparation method of copper/modal fiber composite material |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112530625A (en) * | 2020-11-05 | 2021-03-19 | 青岛大学 | Chitin whisker-based conductive material and preparation method thereof, and aqueous conductive ink and application thereof |
| CN112530625B (en) * | 2020-11-05 | 2022-06-10 | 青岛大学 | Chitin whisker-based conductive material and preparation method thereof, and aqueous conductive ink and application thereof |
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| CN105177538B (en) | 2018-11-23 |
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