CN109837563A - A kind of modified aluminium nitride whisker enhances the preparation method of copper cold screen device - Google Patents
A kind of modified aluminium nitride whisker enhances the preparation method of copper cold screen device Download PDFInfo
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- CN109837563A CN109837563A CN201711226678.1A CN201711226678A CN109837563A CN 109837563 A CN109837563 A CN 109837563A CN 201711226678 A CN201711226678 A CN 201711226678A CN 109837563 A CN109837563 A CN 109837563A
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- cold screen
- screen device
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- zinc
- aluminium nitride
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Abstract
The invention discloses the preparation methods that a kind of aluminium nitride whisker enhances cold screen device, its main feature is that by the way of electroforming while depositing copper device, aluminium nitride whisker is added into electroforming solution, mix whisker uniformly inside alloy, reinforced phase is formed, this method can significantly increase the intensity of copper device.It may finally prepare with some strength, and the cold screen device that wall thickness is very thin；This method solve use copper materials as cold screen device, the problem that product strength is low, easily-deformable；And high-intensitive metal with other, such as nickel, nickel cobalt are compared, and thermal conductivity is much higher by again；Therefore, this method is a kind of preparation method of extraordinary cold screen device.
Description
Technical field
The invention belongs to materials science fields, and in particular to a kind of modified aluminium nitride whisker enhances the system of copper cold screen device
Preparation Method.
Background technique
Integrated Dewar component is the core of infrared detector, and cold screen device is the Primary Component of Dewar component, is to ensure that
Detector works normally one of essential important component in the case where stablizing low temperature.Cold screen be located at Dewar bottle and detector array it
Between, it can extremely efficient shield infrared stray radiation and other electromagnetic wave good fortune are penetrated, reduce the thermic load in Dewar low-temperature working area,
Effectively shorten the cooling activation time, this is very important for improving the response frequency of equipment and shortening the response time.Furthermore
Cold screen can effectively reduce background thermal noise, improve infrared detector to the signal-to-noise ratio of tracking target.
Requirement in use to cold screen device is very high.Firstly, device must have certain intensity, that is, make
With, assembly or heat treatment process in cannot deform；Secondly, device quality wants small, therefore, which is typically all thin-walled devices；
Third, the thermal conductivity of device want high, to shorten the detector cold start-up time.Cold screen device be more likely in the design process using
Therefore fine copper material, but copper intensity itself is not high when material using copper as cold screen, usually selects complicated structure to set
Count or increase cold screen thickness of detector to guarantee the intensity of copper device, but can increase electroforming process complexity and cold screen device
Part quality.Sometimes also the lower nickel cobalt alloy material of thermal conductivity can be selected in order to meet the requirement of thin-walled and intensity.For many years,
Correlative technology field, which always searches for one kind, can either guarantee the performance of device strength and thin-walled, and can take into account the cold of thermal conductivity
Shield device preparation method.This invention, as reinforced phase, increases the strong of thin-walled copper piece using the aluminium nitride whisker of high heat conductance
Degree, while the aluminium nitride of high heat conductance can't be such that the overall thermal conductivity of cold screen device reduces again.
Therefore, the cold screen device of this method preparation will meet simultaneously under the premise of guaranteeing cold screen device thin-walled and intensity
Its requirement to thermal conductivity.
Summary of the invention
The purpose of the present invention is to provide the preparation method that a kind of modified aluminium nitride whisker enhances copper cold screen device,
A kind of modified aluminium nitride whisker enhances the preparation method of copper cold screen device, includes the following steps:
(1) preparation meets the aluminum alloy material core model of cold screen dimensions requirement:
(2) pre-treating aluminium alloy material core model:
(3) the cold screen device of electroforming: being connected to the cathode of DC power supply as electroforming cathode for above-mentioned processed core model, pure
Copper sheet is as electroforming anode；Electroforming solution composition: 150~300g/L of copper sulphate, 40~75g/L of sulfuric acid, aluminium nitride powder 50~
100g/L, room temperature condition, current density are 2~10A/dm2, and the time is 5~10 hours, and movable cathode is used during electroforming
Mode carry out solution stirring；
(4) to the post-processing of cold screen device.
The pretreatment of step (2) the aluminum alloy material core model in turn includes the following steps:
(1) core model oil removing: oil removing is carried out to above-mentioned aluminum alloy material core model using degreasing fluid, is heated using ultrasound bath
Oil removing, except oil temperature is 30~100 DEG C, the oil removing time is 1~90min；
(2) core model hot water wash: by the core model ultrasonic wave water washing after oil removing in step (1), ultrasonic wave water washing temperature is 30
~100 DEG C, 1~90min of washing time；
(3) core model derusts: at room temperature with the HNO3 solution or rust removing solution of 20vol% by step (2) processed core model
Wash 10~15s；
(4) cold water is washed: the core model after step (3) derusting is washed 1min or more with distilled water at room temperature；
(5) core model sinks zinc: zinc is sunk in mandrel surface with the heavy zinc agent of alkalinity, room temperature condition, and heavy 15~30s of zinc time, later
It is rinsed with clear water；
(6) core model moves back zinc: remove the heavy zinc of mandrel surface with the HNO3 of 20vol%, room temperature condition, move back the zinc time 10~
30s is rinsed with clear water later；
(7) the secondary heavy zinc of core model: sinking zinc in mandrel surface with the heavy zinc agent of alkalinity, room temperature condition, sinks 5~15s of zinc time, it
It is rinsed afterwards with clear water；
The step (4) in turn includes the following steps to the post-processing of cold screen device:
(1) clear water is washed: the cold screen device after electroforming is cleaned 1~20min in flowing distilled water；
(2) it demoulds: cold screen device being put into the NaOH solution of 5~40wt% concentration and is completely dissolved to core model, temperature is
20~80 DEG C；
(3) clear water is washed: the cold screen device after demoulding being placed in flowing distilled water and cleans 1~20min；
(4) the cold screen device after demoulding ash disposal: is removed into surface dust, temperature in the HNO3 that concentration is 10~50vol%
Room temperature is spent, the time is 10~15s；
(5) clear water is washed: cleaning 1~20min in flowing distilled water；
(6) it dries: drying 10~100min at a temperature of 60~150 DEG C in an oven, obtaining wall thickness is 0.05~0.2mm's
Cold screen device.
The AlN composite granule that aluminium nitride powder in the step (3) selects BN uniformly to wrap up, powder granularity are controlled 20
~500nm.
The degreasing fluid of core model oil removing uses heated alkaline chemical degreasing liquid.
Beneficial effects of the present invention:
In the production cold screen device process of copper, modified aluminium nitride whisker is mixed in copper, and (modified aluminium nitride refers to nitridation
The aluminium nitride whisker of boron cladding), since aluminium nitride has very high thermal coefficient, crystal whisker materials are strong in reinforcing material
While spending, the thermal coefficient of device can't be reduced.
This method can significantly increase the intensity of copper device；It may finally prepare with some strength, and wall thickness is non-
Often thin cold screen device；This method solve use copper materials as cold screen device, the problem that product strength is low, easily-deformable, and
And the metal with other high intensity, such as nickel, nickel cobalt are compared, thermal conductivity is much higher by again.
Specific embodiment
Embodiment 1
A kind of modified aluminium nitride whisker enhances the preparation method of copper cold screen device, successively prepares in accordance with the following steps:
(1) preparation meets the aluminum alloy material core model of cold screen dimensions requirement.
(2) core model oil removing, solution are heated alkaline chemical degreasing liquid, except oil temperature is 40 DEG C (ultrasound bath heating), when
Between be 10min.
(3) core model hot water wash, 40 DEG C of temperature (ultrasound bath heating), time 10min.
(4) core model derusts, and with HNO3 solution (20vol%), washes 10s at room temperature.
(5) cold water is washed, and washes 5min with distilled water at room temperature.
(6) core model sinks zinc: zinc agent, which is sunk, with commercial available alkaline in mandrel surface sinks zinc, temperature room temperature, and time 30s.
(7) clear water rinses
(8) core model moves back zinc: removing the heavy zinc of mandrel surface, temperature room temperature, time 10s with the HNO3 of 20vol%.
(9) clear water rinses
(10) the secondary heavy zinc of core model: sinking zinc agent with commercial available alkaline and in mandrel surface sink zinc, temperature room temperature, time 15s.
(11) clear water rinses
(12) processed core model: being connected to the cathode of DC power supply by electroforming, and fine copper is anode.Electroforming solution composition: sulphur
Sour copper 300g/L, sulfuric acid 70g/L, aluminium nitride 60g/L, temperature room temperature, current density 3A/dm2, time are 5 hours.
(13) clear water is washed: cleaning 10min in flowing distilled water.
(14) it demoulds: by the good cold screen of electroforming, being put into the NaOH solution of 25wt% concentration and be completely dissolved to core model, temperature
It is 70 DEG C, until core model completely removes.
(15) clear water is washed: cleaning 2min in flowing distilled water.
(16) the cold screen device after demoulding ash disposal: is removed into surface dust, temperature chamber in the HNO3 that concentration is 15vol%
Temperature, time 15s.
(17) clear water is washed: cleaning 5min in flowing distilled water.
(18) it dries: drying 30min at a temperature of 110 DEG C in an oven.Obtain the cold screen device that wall thickness is 0.08mm.
Embodiment 2
A kind of modified aluminium nitride whisker enhances the preparation method of copper cold screen device, successively prepares in accordance with the following steps:
(1) preparation meets the aluminum alloy material core model of cold screen dimensions requirement；
(2) core model oil removing: solution is heated alkaline chemical degreasing liquid, except oil temperature is 60 DEG C (ultrasound bath heating), when
Between be 15min；
(3) core model hot water wash: temperature 60 C (ultrasound bath heating), time 5min.
(4) core model derusts: with commercially available rust removing solution, washing 15s at room temperature.
(5) cold water is washed: washing 5min with distilled water at room temperature.
(6) core model sinks zinc: zinc agent, which is sunk, with commercial available alkaline in mandrel surface sinks zinc, temperature room temperature, and time 20s.
(7) clear water rinses；
(8) core model moves back zinc: removing the heavy zinc of mandrel surface, temperature room temperature, time 15s with the HNO3 of 20vol%.
(9) clear water rinses:
(10) the secondary heavy zinc of core model: sinking zinc agent with commercial available alkaline and in mandrel surface sink zinc, temperature room temperature, time 10s.
(11) clear water rinses；
(12) processed core model: being connected to the cathode of DC power supply by electroforming, and fine copper is anode.Electroforming solution composition: sulphur
Sour copper 275g/L, sulfuric acid 60g/L, aluminium nitride 60g/L, temperature room temperature, current density 5A/dm2, time are 8 hours；
(13) clear water is washed: cleaning 5min in flowing distilled water；
(14) it demoulds: by the good cold screen of electroforming, being put into the NaOH solution of 30wt% concentration and be completely dissolved to core model, temperature
It is 70 DEG C；
(15) clear water is washed: cleaning 3min in flowing distilled water；
(16) the cold screen device after demoulding ash disposal: is removed into surface dust, temperature chamber in the HNO3 that concentration is 30vol%
Temperature, time 15s；
(17) clear water is washed: cleaning 3min in flowing distilled water；
(18) it dries: drying 30min at a temperature of 100 DEG C in an oven；Obtain the cold screen device that wall thickness is 0.9mm.
Claims (5)
1. the preparation method that a kind of modified aluminium nitride whisker enhances copper cold screen device, which comprises the steps of:
(1) preparation meets the aluminum alloy material core model of cold screen dimensions requirement:
(2) pre-treating aluminium alloy material core model:
(3) above-mentioned processed core model the cold screen device of electroforming: is connected to the cathode of DC power supply as electroforming cathode, fine copper plate
As electroforming anode；Electroforming solution composition: 150~300g/L of copper sulphate, 40~75g/L of sulfuric acid, 50~100g/L of aluminium nitride powder,
Room temperature condition, current density are 2~10A/dm2, the time is 5~10 hours, during electroforming by the way of movable cathode
Carry out solution stirring；
(4) post-processing of cold screen device.
2. a kind of modified aluminium nitride whisker according to claim 1 enhances the preparation method of copper cold screen device, feature
It is, the pretreatment of the aluminum alloy material core model in turn includes the following steps:
(1) core model oil removing: oil removing is carried out to above-mentioned aluminum alloy material core model using degreasing fluid, is removed using ultrasound bath heating
Oil, except oil temperature is 30~100 DEG C, the oil removing time is 1~90min；
(2) core model hot water wash: by the core model ultrasonic wave water washing after oil removing in step (1), ultrasonic wave water washing temperature is 30~100
DEG C, 1~90min of washing time；
(3) core model derusts: by the HNO of the processed core model 20vol% of step (2)3Solution or rust removing solution wash 10 at room temperature~
15s；
(4) cold water is washed: the core model after step (3) derusting is washed 1min or more with distilled water at room temperature；
(5) core model sinks zinc: sinking zinc in mandrel surface with the heavy zinc agent of alkalinity, room temperature condition sinks 15~30s of zinc time, later with clearly
Water rinses；
(6) core model moves back zinc: with the HNO of 20vol%3The heavy zinc of mandrel surface is removed, room temperature condition moves back 10~30s of zinc time, it
It is rinsed afterwards with clear water；
(7) the secondary heavy zinc of core model: sinking zinc in mandrel surface with the heavy zinc agent of alkalinity, room temperature condition, sinks zinc time 5~15s, Zhi Houyong
Clear water rinses.
3. a kind of modified aluminium nitride whisker according to claim 1 enhances the preparation method of copper cold screen device, feature
It is, the step (4) in turn includes the following steps to the post-processing of cold screen device:
(1) clear water is washed: the cold screen device after electroforming is cleaned 1~20min in flowing distilled water；
(2) demould: cold screen device is put into the NaOH solution of 5~40wt% concentration and is completely dissolved to core model, temperature be 20~
80℃；
(3) clear water is washed: the cold screen device after demoulding being placed in flowing distilled water and cleans 1~20min；
(4) ash disposal: by the cold screen device after demoulding in the HNO that concentration is 10~50vol%3Middle removing surface dust, temperature chamber
Temperature, time are 10~15s；
(5) clear water is washed: cleaning 1~20min in flowing distilled water；
(6) it dries: drying 10~100min at a temperature of 60~150 DEG C in an oven, obtain the cold screen that wall thickness is 0.05~0.2mm
Device.
4. a kind of modified aluminium nitride whisker according to claim 1 enhances the preparation method of copper cold screen device, feature
Be, the AlN composite granule that aluminium nitride powder in the step (3) selects BN uniformly to wrap up, powder granularity control 20~
500nm。
5. a kind of modified aluminium nitride whisker according to claim 2 enhances the preparation method of copper cold screen device, feature
It is, the degreasing fluid of core model oil removing uses heated alkaline chemical degreasing liquid.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102618894A (en) * | 2012-04-01 | 2012-08-01 | 昆明理工大学 | Method for preparing thin-wall parts by using electroforming nickel-cobalt alloy |
| CN103014819A (en) * | 2011-09-27 | 2013-04-03 | 肖云捷 | Wearable compound layer material for machine parts and manufacturing method and equipment thereof |
-
2017
- 2017-11-29 CN CN201711226678.1A patent/CN109837563B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103014819A (en) * | 2011-09-27 | 2013-04-03 | 肖云捷 | Wearable compound layer material for machine parts and manufacturing method and equipment thereof |
| CN102618894A (en) * | 2012-04-01 | 2012-08-01 | 昆明理工大学 | Method for preparing thin-wall parts by using electroforming nickel-cobalt alloy |
Non-Patent Citations (2)
| Title |
|---|
| 张允诚: "《电镀手册 第二版》", 31 July 1997, 北京：国防工业出版社 * |
| 王海军: "冷屏件电铸设备的应用研究", 《山西电子技术》 * |
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