CN107513639A - A kind of method for preparing the modified Ti W alloys in barrier layer - Google Patents
A kind of method for preparing the modified Ti W alloys in barrier layer Download PDFInfo
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- CN107513639A CN107513639A CN201710871395.6A CN201710871395A CN107513639A CN 107513639 A CN107513639 A CN 107513639A CN 201710871395 A CN201710871395 A CN 201710871395A CN 107513639 A CN107513639 A CN 107513639A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C14/00—Alloys based on titanium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/03—Making non-ferrous alloys by melting using master alloys
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
- C22C27/04—Alloys based on tungsten or molybdenum
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/0094—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with organic materials as the main non-metallic constituent, e.g. resin
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Abstract
The invention discloses a kind of method for preparing the modified Ti W alloys in barrier layer.This method comprises the following steps：Step 1, meter weighs the component of quickening liquid in parts by weight：25 58 parts of polyether sulfone, 14 parts of polyethylene pyrrole network alkanone, 14 parts of polysiloxanes carboxylic acid sodium, 28 parts of dopamine solution；Step 2, Ti W alloys are chosen, after cleaning up, melt to obtain tungsten titanium liquation；Step 3, polyether sulfone and polyethylene pyrrole network alkanone are mixed and is dissolved in polysiloxanes carboxylic acid sodium, heating water bath is incubated 4 6h, adds dopamine solution, 1200 1800rpm speed stirs 20 30min and obtains quickening liquid to after 60 70 DEG C；Step 4, quickening liquid, foam copper and rilanit special are added into tungsten titanium liquation, after stirring, puts into extruder and extrudes modified Ti W.Thermostabilization is good under Ti W alloy high temperature prepared by this method, strong with bipolar adhesive force, and is not easy by other particle contaminants.
Description
Technical field
The invention belongs to thermistor accessory preparation field, and in particular to a kind of barrier layer for preparing is modified Ti-W alloys
Method.
Background technology
With the development of science and technology, the popularization of thermistor uses, barrier layer also turns into more and more important composition portion therewith
Point.Barrier layer is usually other monometallics or binary and ternary alloy three-partalloy, the coating being related in addition to having zinc, nickel, also cobalt, tin,
Ormolu and admiro etc..
Ti-W barrier layers are often used as the barrier layer of bipolar circuit, the metallization structures for using PtSi/Ti-W/Al more, but
PtSi is not sufficiently stable more than 550 DEG C, is contacted more preferably with bipolar, it is necessary to be modified place to existing Ti-W in order that obtaining barrier layer
Reason.In addition, prior art prepares Ti-W barrier layers, although improving adhesive force, barrier layer matter using magnetically controlled sputter method more
Amount is poor, is easily stain by other particulate matters.
The content of the invention
In view of the shortcomings of the prior art, it is an object of the invention to provide a kind of barrier layer for preparing to be modified Ti-W alloys
Method, thermostabilization is good under Ti-W alloy high-temps prepared by this method, strong with bipolar adhesive force, and be not easy to be stained with by other particles
It is dirty.
A kind of method for preparing the modified Ti-W alloys in barrier layer, comprises the following steps：
Step 1, meter weighs the component of quickening liquid in parts by weight：Polyether sulfone 25-58 parts, polyethylene pyrrole network alkanone 1-4 parts,
Polysiloxanes carboxylic acid sodium 1-4 parts, dopamine solution 2-8 parts；
Step 2, Ti-W alloys are chosen, after cleaning up, melt to obtain tungsten titanium liquation；
Step 3, polyether sulfone and polyethylene pyrrole network alkanone are mixed and is dissolved in polysiloxanes carboxylic acid sodium, heating water bath to 60-70
After DEG C, 4-6h is incubated, adds dopamine solution, 1200-1800rpm speed stirring 20-30min obtains quickening liquid；
Step 4, quickening liquid, foam copper and rilanit special are added into tungsten titanium liquation, after stirring, puts into extruder
The middle modified Ti-W of extrusion.
It is the component of quickening liquid in step 1 as improved, meter includes following components in parts by weight：45 parts of polyether sulfone,
3 parts of polyethylene pyrrole network alkanone, 2 parts of polysiloxanes carboxylic acid sodium, 6 parts of dopamine solution.
It is that the dopamine solution is dissolved in 100ml Tri-HCl solution for 120mg dopamine as improved to obtain
The mixed solution arrived.
It is that the molar concentration of the Tri-HCl solution is 5mmolL as improved-1。
It is that tungsten titanium liquation in step 4, quickening liquid, the weight ratio of foam copper and rilanit special are 32- as improved
45:1：12-25:0.8-4.8.
Compared with prior art, the modified Ti-W alloys of the inventive method preparation are simple and easy, low for equipment requirements, by poly-
Foam copper and Ti-W alloy molten solutions are effectively mixed to get modified Ti-W alloys by ether sulfone self-polymeric reaction in dopamine solution, are changed
Property Ti-W alloys and substrate, electrode between Adhesion enhancement, and can use a variety of methods prepare barrier layer, not by magnetic control
The limitation of sputtering method.
Embodiment
The present invention is further described in detail below by specific embodiment.
Embodiment 1
A kind of method for preparing the modified Ti-W alloys in barrier layer, comprises the following steps：
Step 1, meter weighs the component of quickening liquid in parts by weight：25 parts of polyether sulfone, 1 part of polyethylene pyrrole network alkanone, poly- silicon
1 part of oxygen alkane carboxylic acid sodium, 2 parts of dopamine solution；
Step 2, Ti-W alloys are chosen, after cleaning up, melt to obtain tungsten titanium liquation；
Step 3, polyether sulfone and polyethylene pyrrole network alkanone are mixed and is dissolved in polysiloxanes carboxylic acid sodium, heating water bath is to 60 DEG C
Afterwards, 4h is incubated, adds dopamine solution, 1200rpm speed stirring 20min obtains quickening liquid；
Step 4, quickening liquid, foam copper and rilanit special are added into tungsten titanium liquation, after stirring, puts into extruder
The middle modified Ti-W of extrusion.
Wherein, the dopamine solution is that 120mg dopamine is dissolved in the mixing obtained in 100ml Tri-HCl solution
Solution.
The molar concentration of the Tri-HCl solution is 5mmolL-1。
Tungsten titanium liquation in step 4, quickening liquid, the weight ratio of foam copper and rilanit special are 32:1：12:0.8.
Embodiment 2
A kind of method for preparing the modified Ti-W alloys in barrier layer, comprises the following steps：
Step 1, meter weighs the component of quickening liquid in parts by weight：45 parts of polyether sulfone, 3 parts of polyethylene pyrrole network alkanone, poly- silicon
2 parts of oxygen alkane carboxylic acid sodium, 6 parts of dopamine solution；
Step 2, Ti-W alloys are chosen, after cleaning up, melt to obtain tungsten titanium liquation；
Step 3, polyether sulfone and polyethylene pyrrole network alkanone are mixed and is dissolved in polysiloxanes carboxylic acid sodium, heating water bath is to 65 DEG C
Afterwards, 5h is incubated, adds dopamine solution, 1500rpm speed stirring 25min obtains quickening liquid；
Step 4, quickening liquid, foam copper and rilanit special are added into tungsten titanium liquation, after stirring, puts into extruder
The middle modified Ti-W of extrusion.
Wherein, the dopamine solution is that 120mg dopamine is dissolved in the mixing obtained in 100ml Tri-HCl solution
Solution.
The molar concentration of the Tri-HCl solution is 5mmolL-1。
Tungsten titanium liquation in step 4, quickening liquid, the weight ratio of foam copper and rilanit special are 40:1：22:3.2.
Embodiment 3
A kind of method for preparing the modified Ti-W alloys in barrier layer, comprises the following steps：
Step 1, meter weighs the component of quickening liquid in parts by weight：Polyether sulfone 25-58 parts, polyethylene pyrrole network alkanone 1-4 parts,
Polysiloxanes carboxylic acid sodium 1-4 parts, dopamine solution 2-8 parts；
Step 2, Ti-W alloys are chosen, after cleaning up, melt to obtain tungsten titanium liquation；
Step 3, polyether sulfone and polyethylene pyrrole network alkanone are mixed and is dissolved in polysiloxanes carboxylic acid sodium, heating water bath is to 70 DEG C
Afterwards, 6h is incubated, adds dopamine solution, 1800rpm speed stirring 30min obtains quickening liquid；
Step 4, quickening liquid, foam copper and rilanit special are added into tungsten titanium liquation, after stirring, puts into extruder
The middle modified Ti-W of extrusion.
Wherein, the dopamine solution is that 120mg dopamine is dissolved in the mixing obtained in 100ml Tri-HCl solution
Solution.
The molar concentration of the Tri-HCl solution is 5mmolL-1。
Tungsten titanium liquation in step 4, quickening liquid, the weight ratio of foam copper and rilanit special are 45:1：25:4.8.
Embodiment 4
A kind of method for preparing the modified Ti-W alloys in barrier layer, comprises the following steps：
Step 1, meter weighs the component of quickening liquid in parts by weight：25 parts of polyether sulfone, 1 part of polyethylene pyrrole network alkanone, poly- silicon
1 part of oxygen alkane carboxylic acid sodium, 2 parts of dopamine solution；
Step 2, Ti-W alloys are chosen, after cleaning up, melt to obtain tungsten titanium liquation；
Step 3, polyether sulfone and polyethylene pyrrole network alkanone are mixed and is dissolved in polysiloxanes carboxylic acid sodium, heating water bath is to 60 DEG C
Afterwards, 4h is incubated, adds dopamine solution, 1200rpm speed stirring 20min obtains quickening liquid；
Step 4, quickening liquid, foam copper and rilanit special are added into tungsten titanium liquation, after stirring, puts into extruder
The middle modified Ti-W of extrusion.
Wherein, the dopamine solution is that 120mg dopamine is dissolved in the mixing obtained in 100ml Tri-HCl solution
Solution.
The molar concentration of the Tri-HCl solution is 5mmolL-1。
Tungsten titanium liquation in step 4, quickening liquid, the weight ratio of foam copper and rilanit special are 45:1：25:4.8.
By magnetron sputtering method prepared by barrier layer, detection gained barrier layer to modification Ti-W alloys prepared by embodiment 1-4
Performance, as a result as shown in the table, wherein comparative example is Ti-W alloys.
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | |
| Film layer | It is fine and close | It is fine and close | It is fine and close | It is fine and close |
| Surface roughness | It is small | It is small | It is small | It is small |
| Adhesive force/level | 1 | 1 | 1 | 1 |
| TCR after 48h | It is constant | It is constant | It is constant | It is constant |
| TCR (%/K) | 0.2 | 0.6 | 0.4 | 0.5 |
| Homogeneity | It is excellent | It is excellent | It is excellent | It is excellent |
Strengthen with existing Ti-W alloys adhesive ability, and surface roughness is low, TCR value stabilizations, and film layer is fine and close, effectively
Ground plays barrier effect, extends the service life of the electronic devices such as thermistor.
In addition, the invention is not restricted to above-mentioned embodiment, as long as in without departing from the scope of the present invention, can take various
Mode implements the present invention.
Claims (5)
- A kind of 1. method for preparing the modified Ti-W alloys in barrier layer, it is characterised in that comprise the following steps：Step 1, by weight Number meter weighs the component of quickening liquid：Polyether sulfone 25-58 parts, polyethylene pyrrole network alkanone 1-4 parts, polysiloxanes carboxylic acid sodium 1-4 parts, Dopamine solution 2-8 parts；Step 2, Ti-W alloys are chosen, after cleaning up, melt to obtain tungsten titanium liquation；Step 3, by polyether sulfone and The mixing of polyethylene pyrrole network alkanone is dissolved in polysiloxanes carboxylic acid sodium, and heating water bath is incubated 4-6h, adds dopamine to after 60-70 DEG C Solution, 1200-1800rpm speed stirring 20-30min obtain quickening liquid；Step 4, quickening liquid, foam are added into tungsten titanium liquation Copper and rilanit special, after stirring, put into extruder and extrude modified Ti-W.
- 2. according to claim 1 prepare method of the barrier layer with modified Ti-W alloys, it is characterised in that is helped in step 1 The component of plating solution, in parts by weight meter include following components：45 parts of polyether sulfone, 3 parts of polyethylene pyrrole network alkanone, polysiloxanes carboxylic acid 2 parts of sodium, 6 parts of dopamine solution.
- 3. according to claim 2 prepare method of the barrier layer with modified Ti-W alloys, it is characterised in that the dopamine Solution is that 120mg dopamine is dissolved in the mixed solution obtained in 100ml Tri-HCl solution.
- 4. according to claim 3 prepare method of the barrier layer with modified Ti-W alloys, it is characterised in that the Tri- The molar concentration of HCl solution is 5mmolL-1。
- 5. according to claim 1 prepare method of the barrier layer with modified Ti-W alloys, it is characterised in that tungsten in step 4 Titanium liquation, quickening liquid, the weight ratio of foam copper and rilanit special are 32-45:1：12-25:0.8-4.8.
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| CN201710871395.6A CN107513639A (en) | 2017-09-25 | 2017-09-25 | A kind of method for preparing the modified Ti W alloys in barrier layer |
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| CN201710871395.6A CN107513639A (en) | 2017-09-25 | 2017-09-25 | A kind of method for preparing the modified Ti W alloys in barrier layer |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2009534542A (en) * | 2006-04-26 | 2009-09-24 | セントレ・ナショナル・デ・ラ・レシェルシェ・サイエンティフィーク | Nanocrystalline compounds for hydrogen storage |
| CN104611599A (en) * | 2015-01-13 | 2015-05-13 | 西安理工大学 | Preparation method of aplitic tungsten-titanium alloy |
| CN105296777A (en) * | 2015-10-30 | 2016-02-03 | 西安理工大学 | Preparation method for low rich titanium-phase tungsten titanium alloy |
-
2017
- 2017-09-25 CN CN201710871395.6A patent/CN107513639A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2009534542A (en) * | 2006-04-26 | 2009-09-24 | セントレ・ナショナル・デ・ラ・レシェルシェ・サイエンティフィーク | Nanocrystalline compounds for hydrogen storage |
| CN104611599A (en) * | 2015-01-13 | 2015-05-13 | 西安理工大学 | Preparation method of aplitic tungsten-titanium alloy |
| CN105296777A (en) * | 2015-10-30 | 2016-02-03 | 西安理工大学 | Preparation method for low rich titanium-phase tungsten titanium alloy |
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