CN101805522A - Method for preparing copper wax heat sensitive composite material with high heat stability - Google Patents
Method for preparing copper wax heat sensitive composite material with high heat stability Download PDFInfo
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- CN101805522A CN101805522A CN 201010139157 CN201010139157A CN101805522A CN 101805522 A CN101805522 A CN 101805522A CN 201010139157 CN201010139157 CN 201010139157 CN 201010139157 A CN201010139157 A CN 201010139157A CN 101805522 A CN101805522 A CN 101805522A
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Abstract
The invention relates to a method for preparing a copper wax heat sensitive composite material with high heat stability. Micro-nano copper powder particles are mixed with an additive, and then mixed with a microcrystalline wax; when a mass ratio of the micro-nano copper to the microcrystalline wax is 1:4-10:4, the composite material with the high heat stability can be prepared, the speed of thermal response is high and thermal expansivity is high; and the composite material can be used as the heat sensitive material, an expanding material and the like for manufacturing drive elements, transmission elements and control elements, and has wide application and development prospects in engineering.
Description
Technical field
The present invention relates to a kind of preparation method of metal/organic composite material, specifically refer to the preparation method of the high copper wax heat-sensitive composite material of thermostability.
Background technology
Utilize micro-nano metallic particles as strongthener, utilize organic macromolecule/macromolecular compound as body material, the functional composite material of Xing Chenging has been subjected to people's attention like this, obtains to use in growing field.The advantages such as thermal conductivity, electroconductibility and The thermal expansion of polymer of this metal/organic new type functional composite material concurrent metal, and amorphous characteristics are arranged, can be used as temperature sensing material, expanding material etc. in order to make driving, transmission and controlling elements, in engineering, be with a wide range of applications.Present this metal organic composite material has obtained to use widely in departments such as nuclear industry, aerospace industry, national defense industry, industrial or agricultural, and its special importance manifests day by day.Metal/organic new type functional performance of composites can be better than its component materials (material), or have the unexistent performance of former component.
New copper wax heat-sensitive composite material is the product that micro-nano copper powder and macromolecule wax are composited, as temperature sensing material, wherein the wax component has characteristics such as thermal expansivity is good, no fixed configuration, but has the shortcoming of thermal conductivity difference, causes temperature-sensitive device thermal response speed slow; And the heat conductivility of copper is good, therefore considers to add in wax the thermo-sensitive property that copper powder improves wax material.Yet the matrix material that micro-nano metallics and organic compound form, because there is tangible phase interface in these two kinds of storerooms, like this for such material of under the liquid state of being everlasting, working, cause that easily metal reinforcements precipitate and separate from organic basis material comes out, caused such metal organic composite material composite performance instability, even the complex function forfeiture.If the matrix material of this unstable properties is used for heat conduction/conductive element device, can directly influence the stable performance and the work-ing life of components and parts.
Summary of the invention
The technical problem to be solved in the present invention provides the preparation method of the high copper wax heat-sensitive composite material of a kind of thermostability.
Pass through long term studies, now found the method for this material of preparation, micro-nano copper powder particle mixes with additive earlier, mixes with Microcrystalline Wax again, when the ratio of micro-nano copper and Microcrystalline Wax is 1: 4～10: 4 (mass ratio), can make the stronger matrix material of thermostability.
Find in the research, adopt high-energy ball milling method, under nitrogen protection; with micro-nano copper powder particle and additive mixing and ball milling more than 60 hours, with after wax is mixed with into matrix material, thermostability is stronger again; with the increase of ball milling time, the effect that thermostability increases is no longer obvious.
Find also in the research that Yi Yansuan is particularly outstanding for strengthening thermostable effect in the various additives of choosing, when the mass ratio that accounts for described copper powder when Yi Yansuan was 0.5%～10%, this matrix material showed good stabilising effect.
Through the copper wax heat-sensitive composite material that aforesaid method is handled, it is fast not only to have thermal response speed, the characteristics that thermal expansivity is good, and thermostability height.
Embodiment
The following stated describes the present invention in detail.
Among the present invention there be material therefor: copper powder (sieving with 100 order analyses sieve), Microcrystalline Wax (70#), additive has: 4,4-dipyridyl, 2,2-dipyridyl, o-phenanthroline, L-glutamic acid, Threonine, Isoleucine, EDTA, citric acid, Yi Yansuan, phenylformic acid, Whitfield's ointment, stearic acid etc., aspartic acid.
Among the present invention there be used instrument: electronic balance, ball mill, thermal conduction and the hot expansibility detector (patent No.: 200820224260.7).
Thermostability measuring method used among the present invention is: sample hose (the diameter 4cm that a certain amount of sample is added decentralized material thermal conduction and hot expansibility detector, long 40cm) in, controlled temperature is under 80 ℃, in measuring 48 hours, the ratio of the isolating interface of copper wax and testing sample total height (be called for short to separate and compare), separate more unstable more than big more explanation, easy more the separation, thus judge the thermostability performance of such material according to the size of separating ratio.
Comparative Examples
Take by weighing above-mentioned copper powder and put into ball mill, set drum's speed of rotation 200r/min, take out behind the ball milling 72h under nitrogen protection, after stirring than Hybrid Heating by 1: 1 quality with Microcrystalline Wax, measure its thermostability performance, separation is than being 0.150.
Embodiment 1
Take by weighing above-mentioned copper powder and above-mentioned additive; all account for 4% by additive; copper powder accounts for the mixed of 96% (mass ratio); put into ball mill; set drum's speed of rotation 200r/min, under nitrogen protection, take out behind the ball milling 72h, after stirring than Hybrid Heating by 1: 1 quality with Microcrystalline Wax; measure its thermostability performance, the results are shown in Table 1.
The various additives of table 1. separate than table the thermostability copper wax of copper wax material
| Additive | Separate ratio | Additive | Separate ratio | Additive | Separate ratio |
| L-glutamic acid | ??0.056 | ??EDTA | ??0.112 | Phenylformic acid | ??0.038 |
| Threonine | ??0.082 | Citric acid | ??0.147 | Whitfield's ointment | ??0.036 |
| 2, the 2-dipyridyl | ??0.128 | Yi Yansuan | ??0.024 | Stearic acid | ??0.037 |
| 4, the 4-dipyridyl | ??0.112 | Isoleucine | ??0.065 | ||
| O-phenanthroline | ??0.124 | Aspartic acid | ??0.062 |
Embodiment 2
Above-mentioned copper powder and Yi Yansuan are mixed by 96% and 4% mass ratio; put into ball mill; set drum's speed of rotation 200r/min; take out ball milling 12,24,48,72,96,120 backs under nitrogen protection; after stirring than Hybrid Heating by 1: 1 quality with Microcrystalline Wax; measure its thermostability performance, the results are shown in Table 2.
The different ball milling times of table 2. are to the influence of thermal stability
| Ball milling time/h separates ratio | ??12??0.123 | ??24??0.097 | ??48??0.066 | ??72??0.046 | ??96??0.041 | ??120??0.038 |
Embodiment 3
To contain after 4% Yi Yansuan and the 96% copper powder ball milling time in ball mill is 72h, prepare serial copper wax proportioning sample respectively according to the method described above with Microcrystalline Wax again, its ratio is 1: 4,2: 4,3: 4,4: 4,6: 4,8: 4,10: 4, control 80 ℃ of vibration 96h down, measure the thermostability of this series of samples and separate ratio, experimental result sees Table 3.
Table 3. copper wax proportioning and corresponding separation the thereof than table
| Copper: wax | ??1∶4 | ??2∶4 | ??3∶4 | ??4∶4 | ??6∶4 | ??8∶4 | ??10∶4 |
| Separate ratio | ??0.090 | ??0.069 | ??0.057 | ??0.046 | ??0.038 | ??0.034 | ??0.033 |
Embodiment 4
The mass ratio that accounts for copper powder by Yi Yansuan is 0.2%, 0.4%, 0.8%, 1.6%, 2.4%, 3.2%, 4.0% mixing, prepare the serial copper wax matrix material that series contains the different content Yi Yansuan with wax with 3: 2 ratios then, control 80 ℃ of vibration 96h down, measure its thermostability respectively and separate ratio, the results are shown in Table 4.
The separation of table 4. different content Yi Yansuan copper wax matrix material is than table
| Yi Yansuan content | ??0.2％ | ??0.4％ | ??0.8％ | ??1.6％ | ??2.4％ | ??3.2％ | ??4.0％ |
| Separate ratio | ??0.078 | ??0.056 | ??0.045 | ??0.038 | ??0.049 | ??0.061 | ??0.070 |
Claims (5)
1. the preparation method of the copper wax heat-sensitive composite material that a thermostability is high, micro-nano copper powder particle process is with additive blended step;
With Microcrystalline Wax blended step,
It is characterized in that: described micro-nano copper is 1: 4～10: 4 (mass ratio) with the ratio of described Microcrystalline Wax.
2. the preparation method of the copper wax heat-sensitive composite material that thermostability as claimed in claim 1 is high is characterized in that: the step of described micro-nano copper powder particle and additive combination treatment, adopt ball milled that additive and copper powder are handled in nitrogen protection.
3. the preparation method of the copper wax heat-sensitive composite material that thermostability as claimed in claim 2 is high is characterized in that: described ball-milling processing time＞60 hour.
4. the preparation method of the copper wax heat-sensitive composite material that thermostability as claimed in claim 1 is high, it is characterized in that: described additive is 4,4-dipyridyl, 2,2-dipyridyl, o-phenanthroline, L-glutamic acid, Threonine, Isoleucine, EDTA, citric acid, Yi Yansuan, phenylformic acid, Whitfield's ointment, stearic acid, aspartic acid.
5. the preparation method of the copper wax heat-sensitive composite material that thermostability as claimed in claim 4 is high is characterized in that: described additive accounts for the mass ratio 0.2%～10% of described copper powder.
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| CN 201010139157 CN101805522A (en) | 2010-03-31 | 2010-03-31 | Method for preparing copper wax heat sensitive composite material with high heat stability |
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| CN 201010139157 CN101805522A (en) | 2010-03-31 | 2010-03-31 | Method for preparing copper wax heat sensitive composite material with high heat stability |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102166649A (en) * | 2011-01-29 | 2011-08-31 | 浙江工业大学 | Metal/polymer thermosensitive composite |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1830601A (en) * | 2005-03-08 | 2006-09-13 | 东北轻合金有限责任公司 | Ball grinding zinc powder and its manufacturing method |
| CN101265362A (en) * | 2008-05-07 | 2008-09-17 | 曲阜师范大学 | Method for processing function-stable metal organic composite material |
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2010
- 2010-03-31 CN CN 201010139157 patent/CN101805522A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1830601A (en) * | 2005-03-08 | 2006-09-13 | 东北轻合金有限责任公司 | Ball grinding zinc powder and its manufacturing method |
| CN101265362A (en) * | 2008-05-07 | 2008-09-17 | 曲阜师范大学 | Method for processing function-stable metal organic composite material |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102166649A (en) * | 2011-01-29 | 2011-08-31 | 浙江工业大学 | Metal/polymer thermosensitive composite |
| CN102166649B (en) * | 2011-01-29 | 2012-11-21 | 浙江工业大学 | Metal/polymer thermosensitive composite |
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Open date: 20100818 |