CN102560396A - Surface corrosion-resistant low-resistance film and preparation method thereof - Google Patents
Surface corrosion-resistant low-resistance film and preparation method thereof Download PDFInfo
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- CN102560396A CN102560396A CN201110443900XA CN201110443900A CN102560396A CN 102560396 A CN102560396 A CN 102560396A CN 201110443900X A CN201110443900X A CN 201110443900XA CN 201110443900 A CN201110443900 A CN 201110443900A CN 102560396 A CN102560396 A CN 102560396A
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Abstract
The invention discloses a surface corrosion-resistant low-resistance film and a preparation method thereof. The film is coated on the surface of a metal substrate, and comprises metal chromium, a first chromium-carbon mixed layer and a second chromium-carbon mixed layer from inside to outside. The preparation method comprises the following steps of: 1, performing plasma treatment on the metal substrate to enhance the surface activity of the metal substrate; 2, coating metal chromium on the surface of the metal substrate; 3, coating the first chromium-carbon mixed layer outside the metal chromium, and introducing acetylene gas while switching on a target power supply, wherein the content of carbon in a film layer is controlled through the flow of the introduced acetylene; 4, coating the second chromium-carbon mixed layer outside the first chromium-carbon mixed layer, and introducing acetylene gas while switching on a target power supply, wherein the content of carbon in the film layer is controlled through the flow of the introduced acetylene; and 5, after coating of the film layer, stopping heating, naturally cooling to 100 DEG C, and taking out. Due to the adoption of the surface corrosion-resistant low-resistance film, the corrosion resistance of a metal surface is enhanced, the film resistance is low, and the conducting performance of the metal surface is not influenced.
Description
Technical field
The present invention relates to a kind of fuel cell technology field, particularly relate to a kind of surperficial corrosion resistant low-resistance film and preparation method thereof.
Background technology
Metallic corrosion is in the metallic corrosion environment, to have an effect with corrosive medium and make metal become the oxidation shape, and most metal all has corrosion-prone characteristic.The method that increases the erosion resistance of metallic surface at present is through various chemistry or physical means basically, coats the organic or inorganic film in the metallic surface.After this processing, performances such as the conduction of metallic surface, heat conduction receive havoc.Yet under condition restriction such as the environmental protection and the energy, developing various new forms of energy substitute products has become the main flow development trend.Wherein when substitute products such as development of fuel cells, used part core component like pole plate, must be electric, hot good conductor, and corrosion resistance nature will be got well simultaneously.
And to the new demand of fuel battery pole board, the People's Republic of China's patented claim 200810086373.X, No. 200810086375.9 patents disclose schemes such as azote chromium thin film and azote nickel-chromium thin film, and this type of film is to adopt nitriding treatment; And the erosion resistance requirement is high more, and nitrogen content must increase, because the pyridine body is non-conductive; Therefore after nitrogen content increases; Resistance will increase thereupon, and conductivity is affected, and can not satisfy electroconductibility and erosion resistance and require high product simultaneously.
Summary of the invention
The objective of the invention is to overcome the deficiency of prior art, a kind of surperficial corrosion resistant low-resistance film and preparation method thereof is provided, increase the erosion resistance of metallic surface, and sheet resistance is low, does not influence the conductivity of metallic surface.
In order to achieve the above object; The technical scheme that the present invention adopts is: a kind of surperficial corrosion resistant low-resistance film; Plating is in metallic substrate surface; This film comprises chromium metal, the first chromium carbon mixolimnion and the second chromium carbon mixolimnion, and the chromium metal plating is in metallic substrate surface, and the first chromium carbon mixolimnion is between the chromium metal and the second chromium carbon mixolimnion.
Further, the thickness of described chromium metal rete is 30~60 nanometers.
Further, the thicknesses of layers of the described first chromium carbon mixolimnion is 30~60 nanometers, and the content of the chromium of the first chromium carbon mixolimnion is 96%~99%, and surplus is a carbon, more than 2 kinds of compositions overall proportion of accounting for chromium carbon mixolimnion material be 100%.
Further, the thicknesses of layers of the described second chromium carbon mixolimnion is 400~500 nanometers, and the content of the chromium of the second chromium carbon mixolimnion is 80%~90%, and carbon content is 10%~20%, more than 2 kinds of compositions overall proportion of accounting for chromium carbon mixolimnion material be 100%.
A kind of preparation method of surperficial corrosion resistant low-resistance film, described preparing method's step is following:
This preparation method is based on following condition; The vacuum magnetic-control sputtering coating equipment; And coating equipment disposes bias plasma power-supply system, shielding power supply system, target and inserts the sputter gas of Vakuumkammer and the airing system of reactant gases, and sputter gas is an argon gas, and reactant gases is hydrocarbon gas such as acetylene or methane; Metal base places Vakuumkammer, and the vacuum tightness of Vakuumkammer is greater than 1.0 * 10
-3Handkerchief, temperature are 140~160 ℃, and target power supply power is 5~10 kilowatts;
Step 1, metal base is carried out plasma treatment to strengthen the surfactivity of metal base; The bias plasma power source voltage is 1000V~1300V; The dutycycle of pulse square wave is 50%~75%, and the plasma treatment time is 10~15 minutes under the situation of frequency 40Hz;
Step 2, at metallic substrate surface metallizing chromium;
Step 3, outside chromium metal the plating the first chromium carbon mixolimnion; Feed gas acetylene when opening target power supply; The content of carbon is controlled by the flow that feeds acetylene in the rete; The beginning flow is 100 standard ml/min, progressively strengthens the acetylene flow then, and the flow of acetylene reaches 200 standard ml/min in 10 minutes;
Step 4, outside the first chromium carbon mixolimnion plating second chromium carbon mixolimnion, feed gas acetylene when opening target power supply, the content of carbon is controlled by the flow that feeds acetylene in the rete, the constant flow of acetylene is in 180~220 standard ml/min;
After step 5, rete have plated, stop heating, treat that temperature natural is cooled to take out product below 100 ℃.
Further, the thickness of the described chromium metal rete of step 2 is 30~60 nanometers.
Further, the thicknesses of layers of the described first chromium carbon mixolimnion of step 3 is 30~60 nanometers, and the content of the chromium of the first chromium carbon mixolimnion is 96%~99%, and surplus is a carbon, more than 2 kinds of compositions overall proportion of accounting for chromium carbon mixolimnion material be 100%.
Further, the thicknesses of layers of the described second chromium carbon mixolimnion of step 4 is 400~500 nanometers, and the content of the chromium of the second chromium carbon mixolimnion is 80%~90%, and carbon content is 10%~20%, more than 2 kinds of compositions overall proportion of accounting for chromium carbon mixolimnion material be 100%.
Vacuum tightness=atmospheric pressure-psia, vacuum tightness are big more, just represent that psia is more little.
The invention has the beneficial effects as follows: metallizing chromium layer, the first chromium carbon mixolimnion and the second chromium carbon mixolimnion successively on the surface of metal base, can effectively increase the corrosion resistance nature of metallic surface, guarantee that simultaneously its conductivity is unaffected.
Description of drawings
Fig. 1 is a method flow diagram of the present invention.
Embodiment
Purport of the present invention is to provide a kind of preparation method of surperficial corrosion resistant low-resistance film; The anti-corrosion low-resistance film that the present invention designed; Rete is the film group that alternately is formed by stacking chromium and chromium carbon mixture, and its metal base comprises metal and alloys such as stainless steel, aluminium, titanium.Film is for preparing being equipped with on the vacuum magnetic-control sputtering coating equipment of bias plasma power-supply system.The vacuum magnetic-control sputtering plated film must dispose the sputter gas of bias plasma power-supply system, shielding power supply system and target and access Vakuumkammer and the airing system of reactant gases.The sputter gas of indication is an argon gas, and reactant gases is hydrocarbon gas such as acetylene or methane.
Be elaborated with reference to accompanying drawing below in conjunction with embodiment, so that technical characterictic of the present invention and advantage are carried out more deep annotation.
Method flow diagram of the present invention is as shown in Figure 1; A kind of preparation method of surperficial corrosion resistant low-resistance film; This method is described film plated in metallic substrate surface, comprises chromium metal, the first chromium carbon mixolimnion and the second chromium carbon mixolimnion from inside to outside, and described preparing method's step is following:
This preparation method is based on following condition; The vacuum magnetic-control sputtering coating equipment; And coating equipment disposes bias plasma power-supply system, shielding power supply system, target and inserts the sputter gas of Vakuumkammer and the airing system of reactant gases, and sputter gas is an argon gas, and reactant gases is an acetylene; Metal base places Vakuumkammer, and the vacuum tightness of Vakuumkammer is greater than 1.0 * 10
-3Handkerchief, temperature are 140~160 ℃, and target power supply power is 5~10 kilowatts;
Step 1, metal base is carried out plasma treatment to strengthen the surfactivity of metal base; The bias plasma power source voltage is 1000V~1300V; The dutycycle of pulse square wave is 50%~75%, is 10~15 minutes in the situation plasma treatment time of frequency 40Hz;
Step 2, at metallic substrate surface metallizing chromium;
Step 3, outside chromium metal the plating the first chromium carbon mixolimnion; Feed gas acetylene when opening target power supply; The content of carbon is controlled by the flow that feeds acetylene in the rete; The beginning flow is 100 standard ml/min, progressively strengthens the acetylene flow then, and the flow of acetylene reaches 200 standard ml/min in 10 minutes;
Step 4, outside the first chromium carbon mixolimnion plating second chromium carbon mixolimnion, feed gas acetylene when opening target power supply, the content of carbon is controlled by the flow that feeds acetylene in the rete, the constant flow of acetylene is in 180~220 standard ml/min;
After step 5, rete have plated, stop heating, treat that temperature natural is cooled to take out product below 100 ℃.
The thickness of above-mentioned steps 2 described chromium metal retes is 30~60 nanometers.
The thicknesses of layers of the above-mentioned steps 3 described first chromium carbon mixolimnions is 30~60 nanometers, and the content of the chromium of the first chromium carbon mixolimnion is 96%~99%, and surplus is a carbon, more than 2 kinds of compositions overall proportion of accounting for chromium carbon mixolimnion material be 100%.
The thicknesses of layers of the above-mentioned steps 4 described second chromium carbon mixolimnions is 400~500 nanometers, and the content of the chromium of the second chromium carbon mixolimnion is 80%~90%, and carbon content is 10%~20%, more than 2 kinds of compositions overall proportion of accounting for chromium carbon mixolimnion material be 100%.
Vacuum tightness=atmospheric pressure-psia, vacuum tightness are big more, just represent that psia is more little.
Acetylene of the present invention or replace with methane, but the time that needs is more of a specified duration, and the magnetron sputtering target power supply is more powerful.
Corrosion-resistant, low resistance thin film is combined by the rete mutual superposition of three layers of different components, and the first layer is a chromium metal, and thicknesses of layers act as the bonding force that increases rete Cr.C and metal base between 30 to 60 nanometers; The second layer is the first chromium carbon mixolimnion, and thicknesses of layers is between 50 to 100 nanometers, and chromium content is approximately 99%, and carbon content is approximately 1%, act as the transition layer between the second chromium carbon mixolimnion and the metal base; The 3rd layer is the second chromium carbon mixolimnion; But thicknesses of layers is between 400 to 500 nanometers, and chromium content is between 80% to 90%, and carbon content is between 10% to 20%; More than 2 kinds of compositions overall proportion of accounting for chromium carbon mixolimnion be 100%, be the core rete of corrosion resistant low-resistance film combinations.
Corrosion resistant low-resistance film is to prepare being equipped with on the vacuum magnetic-control sputtering coating equipment of bias plasma power-supply system, perhaps realizes with the ion film plating mode.Below in conjunction with embodiment the present invention is made further detailed description.
Embodiment 1
When the surperficial corrosion resistant low-resistance film of preparation; This preparation method is based on following condition, the vacuum magnetic-control sputtering coating equipment, and coating equipment disposes bias plasma power-supply system, shielding power supply system, target and inserts the sputter gas of Vakuumkammer and the airing system of reactant gases; Sputter gas is an argon gas; Reactant gases is an acetylene, and metal base places Vakuumkammer, and the vacuum tightness of Vakuumkammer is greater than 1.0 * 10
-3Handkerchief.
When the temperature of Vakuumkammer is 140 ℃; The magnetron sputtering target power is 5 kilowatts; Metal base is carried out plasma treatment to strengthen the surfactivity of metal base, and the bias plasma power source voltage is 1000V, and the dutycycle of pulse square wave is 50%; At frequency 40Hz, the situation plasma treatment time be 15 minutes; At metallic substrate surface metallizing chromium, the thickness of chromium is 30 nanometers then; At the plating first chromium carbon mixolimnion outside chromium metal, feed gas acetylene when opening target power supply then, the beginning flow is that (sccm is the standard ml/min to 100sccm, and s is the stand standard, under the expression normal conditions; Cc is a milliliter; M is the minute PM).Progressively strengthen the acetylene flow then, the flow of acetylene reaches 200sccm in 10 minutes, and the content of the chromium of the first chromium carbon mixolimnion is 99%, and thicknesses of layers is 30 nanometers; The plating second chromium carbon mixolimnion outside the first chromium carbon mixolimnion feeds gas acetylene when opening target power supply once more, and the content of the chromium of the second chromium carbon mixolimnion is 90%, and the constant flow of acetylene is at 180~220 sccm, and thicknesses of layers is 400 nanometers; After rete has plated, stop heating at last, treat that temperature natural is cooled to take out product below 100 ℃.
Embodiment 2
When the surperficial corrosion resistant low-resistance film of preparation; This preparation method is based on following condition, the vacuum magnetic-control sputtering coating equipment, and coating equipment disposes bias plasma power-supply system, shielding power supply system, target and inserts the sputter gas of Vakuumkammer and the airing system of reactant gases; Sputter gas is an argon gas; Reactant gases is an acetylene, and metal base places Vakuumkammer, and the vacuum tightness of Vakuumkammer is greater than 1.0 * 10
-3Handkerchief.
When the temperature of Vakuumkammer is 150 ℃; The magnetron sputtering target power is 7.5 kilowatts; Metal base is carried out plasma treatment to strengthen the surfactivity of metal base, and the bias plasma power source voltage is 1200V, and the dutycycle of pulse square wave is 60%; At frequency 40Hz, the situation plasma treatment time be 12 minutes; At metallic substrate surface metallizing chromium, the thickness of chromium is 45 nanometers then; The plating first chromium carbon mixolimnion outside chromium metal feeds gas acetylene when opening target power supply then, and the beginning flow is 100sccm; Progressively strengthen the acetylene flow then; The flow of acetylene reaches 200sccm in 10 minutes, and the content of the chromium of the first chromium carbon mixolimnion is 97.5%, and thicknesses of layers is 45 nanometers; The plating second chromium carbon mixolimnion outside the first chromium carbon mixolimnion feeds gas acetylene when opening target power supply once more, and the content of the chromium of the second chromium carbon mixolimnion is 85%, and the constant flow of acetylene is at 180~220 sccm, and thicknesses of layers is 450 nanometers; After rete has plated, stop heating at last, treat that temperature natural is cooled to take out product below 100 ℃.
Embodiment 3
When the surperficial corrosion resistant low-resistance film of preparation; This preparation method is based on following condition, the vacuum magnetic-control sputtering coating equipment, and coating equipment disposes bias plasma power-supply system, shielding power supply system, target and inserts the sputter gas of Vakuumkammer and the airing system of reactant gases; Sputter gas is an argon gas; Reactant gases is an acetylene, and metal base places Vakuumkammer, and the vacuum tightness of Vakuumkammer is greater than 1.0 * 10
-3Handkerchief.
When the temperature of Vakuumkammer is 160 ℃; The magnetron sputtering target power is 10 kilowatts; Metal base is carried out plasma treatment to strengthen the surfactivity of metal base, and the bias plasma power source voltage is 1300V, and the dutycycle of pulse square wave is 70%; At frequency 40Hz, the situation plasma treatment time be 10 minutes; At metallic substrate surface metallizing chromium, the thickness of chromium is 60 nanometers then; At the plating first chromium carbon mixolimnion outside chromium metal, feed gas acetylene when opening target power supply then, the beginning flow is 100sccm; Progressively strengthen the acetylene flow then; The flow of acetylene reaches 200sccm in 10 minutes, and the content of the chromium of the first chromium carbon mixolimnion is 96%, and thicknesses of layers is 60 nanometers; Outside the first chromium carbon mixolimnion, plate the second chromium carbon mixolimnion once more; Feed gas acetylene when opening target power supply, the content of the chromium of the second chromium carbon mixolimnion is 80%, and the constant flow of acetylene is at 180~220 sccm; Thicknesses of layers is 500 nanometers; After rete has plated, stop heating at last, treat that temperature natural is cooled to take out product below 100 ℃.
To sum up; Among the embodiment 1,2,3, in the preparation process of chromium metal, the first chromium carbon mixolimnion and the second chromium carbon mixolimnion, under the certain situation of preparation time; Reaction gas flow and magnetron sputtering target power there are differences, and then the content of chromium is different in the chromium carbon mixolimnion.Reaction gas flow is constant, and target power supply power is big more, and the content of chromium is high more.Otherwise the magnetron sputtering target power is constant, and reaction gas flow is big more, and carbon content is just high more.If limiting time not, then the coating time long more, rete is thick more.
The content of mentioning in the foregoing description is not to be to qualification of the present invention, and under the prerequisite that does not break away from inventive concept of the present invention, any conspicuous replacement is all within protection scope of the present invention.
Claims (8)
1. surperficial corrosion resistant low-resistance film; Plating is characterized in that in metallic substrate surface this film comprises chromium metal, the first chromium carbon mixolimnion and the second chromium carbon mixolimnion; The chromium metal plating is in metallic substrate surface, and the first chromium carbon mixolimnion is between the chromium metal and the second chromium carbon mixolimnion.
2. surperficial corrosion resistant low-resistance film according to claim 1, it is characterized in that: the thickness of described chromium metal rete is 30~60 nanometers.
3. surperficial corrosion resistant low-resistance film according to claim 1; It is characterized in that: the thicknesses of layers of the described first chromium carbon mixolimnion is 30~60 nanometers; The content of the chromium of the first chromium carbon mixolimnion is 96%~99%; Surplus is a carbon, more than 2 kinds of compositions overall proportion of accounting for chromium carbon mixolimnion material be 100%.
4. surperficial corrosion resistant low-resistance film according to claim 1; It is characterized in that: the thicknesses of layers of the said second chromium carbon mixolimnion is 400~500 nanometers; The content of the chromium of the second chromium carbon mixolimnion is 80%~90%; Carbon content is 10%~20%, more than 2 kinds of compositions overall proportion of accounting for chromium carbon mixolimnion material be 100%.
5. a preparation method who realizes each described surperficial corrosion resistant low-resistance film in the claim 1~4 is characterized in that, described preparing method's step is following:
This preparation method is based on following condition; The vacuum magnetic-control sputtering coating equipment; And coating equipment disposes bias plasma power-supply system, shielding power supply system, target and inserts the sputter gas of Vakuumkammer and the airing system of reactant gases, and sputter gas is an argon gas, and reactant gases is hydrocarbon gas such as acetylene or methane); Metal base places Vakuumkammer, and the vacuum tightness of Vakuumkammer is greater than 1.0 * 10
-3Handkerchief, temperature are 140~160 ℃, and target power supply power is 5~10 kilowatts;
Step 1, metal base is carried out plasma treatment to strengthen the surfactivity of metal base; The bias plasma power source voltage is 1000V~1300V; The dutycycle of pulse square wave is 50%~75%, and the plasma treatment time is 10~15 minutes under the situation of frequency 40Hz;
Step 2, at metallic substrate surface metallizing chromium;
Step 3, outside chromium metal the plating the first chromium carbon mixolimnion; Feed gas acetylene when opening target power supply; The content of carbon is controlled by the flow that feeds acetylene in the rete; The beginning flow is 100 standard ml/min, progressively strengthens the acetylene flow then, and the flow of acetylene reaches 200 standard ml/min in 10 minutes;
Step 4, outside the first chromium carbon mixolimnion plating second chromium carbon mixolimnion, feed gas acetylene when opening target power supply, the content of carbon is controlled by the flow that feeds acetylene in the rete, the constant flow of acetylene is in 180~220 standard ml/min;
After step 5, rete have plated, stop heating, treat that temperature natural is cooled to take out product below 100 ℃.
6. the preparation method of surperficial corrosion resistant low-resistance film according to claim 5 is characterized in that: the thickness of the described chromium metal rete of step 2 is 30~60 nanometers.
7. the preparation method of surperficial corrosion resistant low-resistance film according to claim 5; It is characterized in that: the thicknesses of layers of the described first chromium carbon mixolimnion of step 3 is 30~60 nanometers; The content of the chromium of the first chromium carbon mixolimnion is 96%~99%; Surplus is a carbon, more than 2 kinds of compositions overall proportion of accounting for chromium carbon mixolimnion material be 100%.
8. the preparation method of surperficial corrosion resistant low-resistance film according to claim 5; It is characterized in that: the thicknesses of layers of the described second chromium carbon mixolimnion of step 4 is 400~500 nanometers; The content of the chromium of the second chromium carbon mixolimnion is 80%~90%; Carbon content is 10%~20%, more than 2 kinds of compositions overall proportion of accounting for chromium carbon mixolimnion material be 100%.
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Cited By (7)
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CN102800871A (en) * | 2012-08-14 | 2012-11-28 | 上海交通大学 | Fuel cell metal bipolar plate carbon chromium gradient coating and preparation method |
CN103806007A (en) * | 2014-02-21 | 2014-05-21 | 南京航空航天大学 | Pretreatment method for preventing cold-bending cracking of austenitic stainless steel and improving corrosion resistance |
CN103903670A (en) * | 2014-03-24 | 2014-07-02 | 大连理工常州研究院有限公司 | Nickel-based electrical connector and manufacture method thereof |
CN103903669A (en) * | 2014-03-24 | 2014-07-02 | 大连理工常州研究院有限公司 | Copper-based electrical connector and manufacturing method thereof |
CN104313567A (en) * | 2014-09-12 | 2015-01-28 | 湖州鑫隆镀膜科技有限公司 | Metal chromium production technology for replacing electroplating technology |
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CN101517121A (en) * | 2006-07-13 | 2009-08-26 | 梯尔镀层有限公司 | Coating apparatus and method |
CN101257118A (en) * | 2007-05-28 | 2008-09-03 | 大连理工大学 | Double polar plates for fuel battery and method for making surface carbon chromium thin film |
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CN102800871A (en) * | 2012-08-14 | 2012-11-28 | 上海交通大学 | Fuel cell metal bipolar plate carbon chromium gradient coating and preparation method |
CN102800871B (en) * | 2012-08-14 | 2015-07-08 | 上海交通大学 | Fuel cell metal bipolar plate carbon chromium gradient coating and preparation method |
CN103806007A (en) * | 2014-02-21 | 2014-05-21 | 南京航空航天大学 | Pretreatment method for preventing cold-bending cracking of austenitic stainless steel and improving corrosion resistance |
CN103806007B (en) * | 2014-02-21 | 2015-10-28 | 南京航空航天大学 | The pretreatment process of prevention austenitic stainless steel cold bend cracking and raising corrosion resisting property |
CN103903670A (en) * | 2014-03-24 | 2014-07-02 | 大连理工常州研究院有限公司 | Nickel-based electrical connector and manufacture method thereof |
CN103903669A (en) * | 2014-03-24 | 2014-07-02 | 大连理工常州研究院有限公司 | Copper-based electrical connector and manufacturing method thereof |
CN104313567A (en) * | 2014-09-12 | 2015-01-28 | 湖州鑫隆镀膜科技有限公司 | Metal chromium production technology for replacing electroplating technology |
CN108390075A (en) * | 2018-01-24 | 2018-08-10 | 上海交通大学 | Anticorrosive conductive film and its pulsed bias replace magnetron sputtering deposition methods and applications |
CN108390075B (en) * | 2018-01-24 | 2019-04-02 | 上海交通大学 | Anticorrosive conductive film and its pulsed bias alternating magnetron sputtering deposition method and application |
WO2019144853A1 (en) * | 2018-01-24 | 2019-08-01 | 上海交通大学 | Corrosion-resistant conductive film, and pulsed bias voltage alternate magnetron sputtering deposition method and application thereof |
US11634808B2 (en) * | 2018-01-24 | 2023-04-25 | Shanghai Jiaotong University | Anti-corrosion conductive film and pulse bias alternation-based magnetron sputtering deposition method and application thereof |
WO2022084519A1 (en) | 2020-10-23 | 2022-04-28 | Université De Namur | Tunable multifunctional carbon-based coatings |
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Application publication date: 20120711 |