CN105483611A - Preparation method of beryllium copper alloy surface Ti+N/Ti composite cementation layer - Google Patents
Preparation method of beryllium copper alloy surface Ti+N/Ti composite cementation layer Download PDFInfo
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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Abstract
The invention discloses a preparation method of a beryllium copper alloy surface Ti+N/Ti composite cementation layer, belongs to the technical field of metal material surface modification. The preparation method comprises the steps that (1) a beryllium copper alloy workpiece is pretreated; (2) a plasma titanizing process is carried out in a plasma surface alloying furnace; and (3) after plasma titanizing, Ti+N co-cementation is carried out continuously, and through plasma tetanizing and Ti+N co-cementation treatment, the beryllium copper alloy surface Ti+N/Ti composite cementation layer is obtained finally. According to the preparation method, the plasma surface alloying technology is combined with an ion nitriding technology, the Ti+N/Ti composite cementation layer is formed on the surface of a soft beryllium copper alloy, and the obtained composite cementation layer has good abrasion resistance.
Description
Technical field
The present invention relates to the preparation method of a kind of beryllium copper surface Ti+N/Ti compisite seeping layer, belong to technical field of metal material surface modification.
Background technology
Beryllium copper, due to advantages such as its good conduction, thermal conductivity, higher elastic limits, is widely used in the multiple fields such as electronic apparatus, aerospace, petrochemical complex, has become indispensable essential industry material in the development of the national economy.Because the hardness of QBe1.9 alloy is low, wear no resistance, for the beryllium copper part for friction environment as gear, test probe, shell fragment etc., often can because its hardness is low serious wear.Thermal treatment is the main method improving QBe1.9 alloy mechanical property at present.But being subject to the restriction of QBe1.9 alloying constituent, structure etc., after thermal treatment, beryllium copper hardness increase rate is limited, not obvious to the improvement result of wear resistance.
TiN has high rigidity, low-friction coefficient and good wear resistance and erosion resistance, is the good material preparing hard top layer.With regard to beryllium copper, because its matrix is softer, be difficult to support hard TiAlN thin film on it, the bonding force in addition between TiAlN thin film and matrix is more weak, directly prepares the improvement result of ganoine thin film to wear resistance very little on beryllium copper surface.
Summary of the invention
The object of the invention is to overcome the limitation directly preparing ganoine thin film at soft matrix surface, a kind of preparation method forming the compisite seeping layer containing hard Ti+N and Ti on beryllium copper surface is provided, plasma surface-alloying process is combined with ion nitriding technology, form Ti+N/Ti compisite seeping layer on soft beryllium copper surface, the compisite seeping layer obtained has good wear resistance.
The preparation method of a kind of beryllium copper surface provided by the invention Ti+N/Ti compisite seeping layer, comprises the following steps:
(1) beryllium copper workpiece pre-treatment: beryllium copper workpiece surface is washed sand papering → bortz powder polishing → acetone cleaning through SiC, for subsequent use after dry;
(2) pretreated beryllium copper workpiece is placed on the negative electrode backing plate in plasma surface alloying stove, and around it, adds an auxiliary cathode, auxiliary cathode is provided with hole; Titanium board is placed on above beryllium copper workpiece by target cathode, and Titanium board is positioned at auxiliary cathode, with beryllium copper workpiece spacing 15 ~ 25mm;
(3) beryllium copper workpiece is connected with workpiece power supply, becomes workpiece pole, then Titanium board is connected with target power supply by target cathode frame, become source electrode;
(4) plasma surface alloying stove is evacuated to highest attainable vacuum, passes into argon gas, connect workpiece power supply, produce geseous discharge, ion bombardment beryllium copper workpiece 10 ~ 20min, operating air pressure is 20 ~ 50Pa;
(5) titanium target power supply is connected, hollow cathode effect is produced at workpiece and source electrode two interpolar, when temperature is increased to 750 ~ 900 DEG C, keep operating air pressure 30 ~ 50Pa, under workpiece and source voltage are respectively 300 ~ 500V and 580 ~ 800V condition, start the preparation carrying out beryllium copper surface titanium alloy layer, oozing the titanium time is 0.5 ~ 3h;
(6) ooze after titanium terminates, be filled with ammonia, adjusting gas flow makes Ar:NH
3volume ratio be 5:3 ~ 5, air pressure is 70 ~ 100Pa, and oozing temperature is altogether 750 ~ 900 DEG C, and workpiece voltage is 550 ~ 700V, source voltage is 800 ~ 950V, after oozing 1 ~ 3h altogether, maintains normal glow discharge cooling 0.5 ~ 1h, deenergization, cuts out gas, cools to room temperature with the furnace; Obtain beryllium copper Ti+N/Ti compisite seeping layer.
Preferably, the preparation method of described beryllium copper surface Ti+N/Ti compisite seeping layer, comprises the following steps:
(1) beryllium copper workpiece pre-treatment: beryllium copper workpiece surface is washed sand papering → bortz powder polishing → acetone cleaning through SiC, for subsequent use after dry;
(2) pretreated beryllium copper workpiece is placed on the negative electrode backing plate in plasma surface alloying stove, and around it, adds an auxiliary cathode, auxiliary cathode is provided with hole; Titanium board is placed on above beryllium copper workpiece by target cathode, and Titanium board is positioned at auxiliary cathode, with beryllium copper workpiece spacing 18 ~ 22mm;
(3) beryllium copper workpiece is connected with workpiece power supply, becomes workpiece pole, then Titanium board is connected with target power supply by target cathode frame, become source electrode;
(4) plasma surface alloying stove is evacuated to highest attainable vacuum, passes into argon gas, connect workpiece power supply, produce geseous discharge, ion bombardment beryllium copper workpiece 15 ~ 18min, operating air pressure is 30 ~ 40Pa;
(5) titanium target power supply is connected, hollow cathode effect is produced at workpiece and source electrode two interpolar, when temperature is increased to 830 ~ 860 DEG C, keep operating air pressure 33 ~ 38Pa, under workpiece and source voltage are respectively 350 ~ 400V and 600 ~ 700V condition, start the preparation carrying out beryllium copper surface titanium alloy layer, oozing the titanium time is 1.5 ~ 2.5h;
(6) ooze after titanium terminates, be filled with ammonia, adjusting gas flow makes Ar:NH
3volume ratio be 5:3 ~ 4, air pressure is 75 ~ 90Pa, and oozing temperature is altogether 830 ~ 880 DEG C, and workpiece voltage is 600 ~ 650V, source voltage is 850 ~ 900V, after oozing 1.5 ~ 2.5h altogether, maintains normal glow discharge cooling 0.5 ~ 1h, deenergization, cuts out gas, cools to room temperature with the furnace; Obtain beryllium copper Ti+N/Ti compisite seeping layer.
In above-mentioned preparation method, the structure of described plasma surface alloying stove is as follows:
Furnace shell is cylindrical structural, in furnace shell, center is provided with workpiece negative electrode, it is negative electrode backing plate above workpiece negative electrode, beryllium copper workpiece is positioned at negative electrode backing plate center upper portion, be provided with tubular auxiliary cathode above negative electrode backing plate workpiece is placed in one, in 10cm place processing 3-φ 8mm hole above auxiliary cathode, for passing into argon gas, in 25cm place processing φ 20mm hole below auxiliary cathode, it is ammonia inlet mouth; Be provided with the Titanium board be connected with target cathode frame above beryllium copper workpiece, Titanium board is positioned at auxiliary cathode, is 15 ~ 25mm with the spacing of beryllium copper workpiece; Beryllium copper workpiece is connected with workpiece power supply, becomes workpiece pole, and Titanium board is connected with target power supply by target cathode frame, becomes source electrode; Drop-bottom perforate connects source of the gas and vacuum extractor respectively.
Of the present invention
beneficial effect:
Titanium is oozed and Ti+N oozes process altogether, at beryllium copper surface preparation Ti+N/Ti compisite seeping layer by plasma.Ooze the tissue distribution that rear surface forms rich TiN layer/TiN+Ti+Cu+Be layer/Ti+Cu+Be layer/matrix altogether, wherein, the interface between infiltration layer with infiltration layer, between infiltration layer with matrix is connected with diffusion layer, has good bonding strength.Rich Ti+N top layer maintains the premium propertiess such as TiN height is hard, wear-resisting, the TiN+Ti+Cu+Be diffusion transition layer formed between matrix and top layer strengthens the comprehensive load capacity of matrix to the rich TiN top layer of hard, make beryllium copper wear resistance be improved significantly, significant to the application of widening beryllium copper.
Accompanying drawing explanation
Fig. 1 is the structural representation of plasma surface alloying furnace apparatus;
Fig. 2 is that after beryllium copper oozes titanium and Ti+N/Ti composite cementation, alloying element distributes along infiltration layer;
Fig. 3 is the frictional coefficient figure after beryllium copper base material and Ti+N/Ti composite cementation;
Fig. 4 is the specific wear rate figure after beryllium copper base material and Ti+N/Ti composite cementation.
In figure: 1-furnace shell, 2-auxiliary cathode, 3-Titanium board, 4-ammonia inlet mouth, 5-beryllium copper workpiece, 6-negative electrode backing plate, 7-drop-bottom, 8-aeration aperture, 9-workpiece negative electrode, 10-aspirating hole, 11-target cathode frame, 12-workpiece power supply, 13-target power supply.
Embodiment
Further illustrate the present invention below by embodiment, but be not limited to following examples.
First the processing unit that the present invention uses is illustrated as follows:
As shown in Figure 1, the structure of the plasma surface alloying stove of the present invention's employing is as follows:
Furnace shell 1 is cylindrical structural, in furnace shell 1, center is provided with workpiece negative electrode 9, it is negative electrode backing plate 6 above workpiece negative electrode 9, beryllium copper workpiece 5 is positioned at negative electrode backing plate 6 center upper portion, tubular auxiliary cathode 2 is provided with, in 10cm place processing 3-φ 8mm hole above auxiliary cathode 2, for passing into argon gas above negative electrode backing plate 6, in 25cm place processing φ 20mm hole below auxiliary cathode 2, it is ammonia inlet mouth 4; Be provided with the Titanium board 3 be connected with target cathode frame 11 above beryllium copper workpiece 5, Titanium board 3 is positioned at auxiliary cathode 2, and Titanium board 3 and beryllium copper workpiece 5 spacing are 15 ~ 25mm; Beryllium copper workpiece 5 is connected with workpiece power supply 12, becomes workpiece pole, and Titanium board 3 is connected with target power supply 13 by target cathode frame 11, becomes source electrode; Drop-bottom 7 is respectively equipped with aeration aperture 8 and aspirating hole 10, and aeration aperture 8 connects source of the gas, and aspirating hole 10 connects vacuum extractor.
Embodiment 1:
The preparation method of the beryllium copper surface Ti+N/Ti compisite seeping layer that the present embodiment provides, comprises the following steps:
(1) beryllium copper workpiece pre-treatment: beryllium copper workpiece surface is washed sand papering → bortz powder polishing → acetone cleaning through SiC, for subsequent use after dry;
(2) pretreated beryllium copper workpiece 5 is placed on the negative electrode backing plate 6 in plasma surface alloying stove, and around it, adds an auxiliary cathode 2, auxiliary cathode processes hole, is convenient to working gas and passes into; Titanium board 3 is placed in above beryllium copper workpiece by target cathode frame 11, and Titanium board 3 is positioned at auxiliary cathode, with beryllium copper workpiece spacing 18mm;
Target selects purity to be the Titanium board of 99.9%;
(3) beryllium copper workpiece is connected with workpiece power supply 12, becomes workpiece pole, then Titanium board is connected with target power supply 13 by target cathode frame, become source electrode;
(4) plasma surface alloying stove is evacuated to highest attainable vacuum 10
-2pa, passes into argon gas, connects workpiece power supply, and produce geseous discharge, ion bombardment beryllium copper workpiece 15min, operating air pressure is 50Pa;
(5) titanium target power supply is connected, hollow cathode effect is produced at workpiece and target two interpolar, when temperature is increased to 880 DEG C, keep operating air pressure 50Pa, under workpiece and source voltage are respectively 490V and 780V condition, start the preparation carrying out beryllium copper surface titanium alloy layer, ooze titanium time 1.5h;
(6) ooze after titanium terminates, be filled with ammonia, adjusting gas flow makes Ar:NH
3=5:4, air pressure is 100Pa, and oozing temperature is altogether 880 DEG C, and workpiece voltage is 660V, and source voltage is 900V, and after oozing 2h altogether, maintain normal glow discharge cooling 1h, deenergization, cuts out gas, cool to room temperature with the furnace; Obtain beryllium copper Ti+N/Ti compisite seeping layer.
(7) specific wear rate detection is carried out to the beryllium copper Ti+N/Ti compisite seeping layer obtained, and contrast with untreated titanium alloy workpiece.
Under above-mentioned processing condition, can at the wear-resisting Ti+N/Ti compisite seeping layer of beryllium copper surface preparation.Fig. 2 is QBe1.9 alloy surface alloy layer composition profiles after Ti+N/Ti composite cementation, illustrates at the compisite seeping layer of beryllium copper surface formation containing Ti+N/Ti.Fig. 3,4 displays, after the process of Ti+N/Ti composite cementation, beryllium copper surface ratio wear rate and frictional coefficient, all far below untreated beryllium copper base material, have good wear-resisting and antifriction performance.
Embodiment 2:
The preparation method of the beryllium copper surface Ti+N/Ti compisite seeping layer that the present embodiment provides, comprises the following steps:
(1) beryllium copper workpiece pre-treatment: beryllium copper workpiece surface is washed sand papering → bortz powder polishing → acetone cleaning through SiC, for subsequent use after dry;
(2) pretreated beryllium copper workpiece 5 is placed on the negative electrode backing plate 6 in plasma surface alloying stove, and around it, adds an auxiliary cathode 2, auxiliary cathode processes hole, is convenient to working gas and passes into; Titanium board 3 is placed in above beryllium copper workpiece by target cathode frame 11, and Titanium board 3 is positioned at auxiliary cathode, with beryllium copper workpiece spacing 18mm;
Target selects purity to be the Titanium board of 99.9%;
(3) beryllium copper workpiece is connected with workpiece power supply 12, becomes workpiece pole, then Titanium board is connected with target power supply 13 by target cathode frame, become source electrode;
(4) plasma surface alloying stove is evacuated to highest attainable vacuum 10
-2pa, passes into argon gas, connects workpiece power supply, and produce geseous discharge, ion bombardment beryllium copper workpiece 15min, operating air pressure is 35Pa;
(5) titanium target power supply is connected, hollow cathode effect is produced at workpiece and target two interpolar, when temperature is increased to 830 DEG C, keep operating air pressure 35Pa, under workpiece and source voltage are respectively 450V and 700V condition, start the preparation carrying out beryllium copper surface titanium alloy layer, ooze titanium time 3h;
(6) ooze after titanium terminates, be filled with ammonia, adjusting gas flow makes Ar:NH
3=5:3, air pressure is 85Pa, and oozing temperature is altogether 850 DEG C, and workpiece voltage is 630V, and source voltage is 870V, and after oozing 2h altogether, maintain normal glow discharge cooling 0.6h, deenergization, cuts out gas, cool to room temperature with the furnace; Obtain beryllium copper Ti+N/Ti compisite seeping layer.
(7) specific wear rate detection is carried out to the beryllium copper TiN/Ti infiltration layer obtained, and contrast with untreated titanium alloy workpiece.
Under above-mentioned processing condition, can at the wear-resisting Ti+N/Ti compisite seeping layer of beryllium copper surface preparation.Fig. 3,4 displays, after the process of Ti+N/Ti composite cementation, beryllium copper surface ratio wear rate and frictional coefficient, all far below untreated beryllium copper base material, have good wear-resisting and antifriction performance.
Embodiment 3:
The preparation method of the beryllium copper surface Ti+N/Ti compisite seeping layer that the present embodiment provides, comprises the following steps:
(1) beryllium copper workpiece pre-treatment: beryllium copper workpiece surface is washed sand papering → bortz powder polishing → acetone cleaning through SiC, for subsequent use after dry;
(2) pretreated beryllium copper workpiece 5 is placed on the negative electrode backing plate 6 in plasma surface alloying stove, and around it, adds an auxiliary cathode 2, auxiliary cathode processes hole, is convenient to working gas and passes into; Titanium board 3 is placed in above beryllium copper workpiece by target cathode frame 11, and Titanium board 3 is positioned at auxiliary cathode, with beryllium copper workpiece spacing 18mm;
Target selects purity to be the Titanium board of 99.9%;
(3) beryllium copper workpiece is connected with workpiece power supply 12, becomes workpiece pole, then Titanium board is connected with target power supply 13 by target cathode frame, become source electrode;
(4) plasma surface alloying stove is evacuated to highest attainable vacuum 10
-2pa, passes into argon gas, connects workpiece power supply, and produce geseous discharge, ion bombardment beryllium copper workpiece 20min, operating air pressure is 25Pa;
(5) titanium target power supply is connected, hollow cathode effect is produced at workpiece and target two interpolar, when temperature is increased to 750 DEG C, keep operating air pressure 30Pa, under workpiece and source voltage are respectively 300V and 580V condition, start the preparation carrying out beryllium copper surface titanium alloy layer, ooze titanium time 3h;
(6) ooze after titanium terminates, be filled with ammonia, adjusting gas flow makes Ar:NH
3=5:5, air pressure is 76Pa, and oozing temperature is altogether 750 DEG C, and workpiece voltage is 570V, and source voltage is 820V, and after oozing 3h altogether, maintain normal glow discharge cooling 0.5h, deenergization, cuts out gas, cool to room temperature with the furnace; Obtain beryllium copper Ti+N/Ti compisite seeping layer.
(7) specific wear rate detection is carried out to the beryllium copper TiN/Ti infiltration layer obtained, and contrast with untreated titanium alloy workpiece.
Under above-mentioned processing condition, can at the wear-resisting Ti+N/Ti compisite seeping layer of beryllium copper surface preparation.Fig. 3,4 displays, after the process of Ti+N/Ti composite cementation, beryllium copper surface ratio wear rate and frictional coefficient, all far below untreated beryllium copper base material, have good wear-resisting and antifriction performance.
Claims (3)
1. a preparation method for beryllium copper surface Ti+N/Ti compisite seeping layer, is characterized in that: comprise the following steps:
(1) beryllium copper workpiece pre-treatment: beryllium copper workpiece surface is washed sand papering → bortz powder polishing → acetone cleaning through SiC, for subsequent use after dry;
(2) pretreated beryllium copper workpiece is placed on the negative electrode backing plate in plasma surface alloying stove, and around it, adds an auxiliary cathode, auxiliary cathode is provided with hole; Titanium board is placed on above beryllium copper workpiece by target cathode, and Titanium board is positioned at auxiliary cathode, with beryllium copper workpiece spacing 15 ~ 25mm;
(3) beryllium copper workpiece is connected with workpiece power supply, becomes workpiece pole, then Titanium board is connected with target power supply by target cathode frame, become source electrode;
(4) plasma surface alloying stove is evacuated to highest attainable vacuum, passes into argon gas, connect workpiece power supply, produce geseous discharge, ion bombardment beryllium copper workpiece 10 ~ 20min, operating air pressure is 20 ~ 50Pa;
(5) titanium target power supply is connected, hollow cathode effect is produced at workpiece and source electrode two interpolar, when temperature is increased to 750 ~ 900 DEG C, keep operating air pressure 30 ~ 50Pa, under workpiece and source voltage are respectively 300 ~ 500V and 580 ~ 800V condition, start the preparation carrying out beryllium copper surface titanium alloy layer, oozing the titanium time is 0.5 ~ 3h;
(6) ooze after titanium terminates, be filled with ammonia, adjusting gas flow makes Ar:NH
3volume ratio be 5:3 ~ 5, air pressure is 70 ~ 100Pa, and oozing temperature is altogether 750 ~ 900 DEG C, and workpiece voltage is 550 ~ 700V, source voltage is 800 ~ 950V, after oozing 1 ~ 3h altogether, maintains normal glow discharge cooling 0.5 ~ 1h, deenergization, cuts out gas, cools to room temperature with the furnace; Obtain beryllium copper Ti+N/Ti compisite seeping layer.
2. the preparation method of beryllium copper surface according to claim 1 Ti+N/Ti compisite seeping layer, is characterized in that: comprise the following steps:
(1) beryllium copper workpiece pre-treatment: beryllium copper workpiece surface is washed sand papering → bortz powder polishing → acetone cleaning through SiC, for subsequent use after dry;
(2) pretreated beryllium copper workpiece is placed on the negative electrode backing plate in plasma surface alloying stove, and around it, adds an auxiliary cathode, auxiliary cathode is provided with hole; Titanium board is placed on above beryllium copper workpiece by target cathode, and Titanium board is positioned at auxiliary cathode, with beryllium copper workpiece spacing 18 ~ 22mm;
(3) beryllium copper workpiece is connected with workpiece power supply, becomes workpiece pole, then Titanium board is connected with target power supply by target cathode frame, become source electrode;
(4) plasma surface alloying stove is evacuated to highest attainable vacuum, passes into argon gas, connect workpiece power supply, produce geseous discharge, ion bombardment beryllium copper workpiece 15 ~ 18min, operating air pressure is 30 ~ 40Pa;
(5) titanium target power supply is connected, hollow cathode effect is produced at workpiece and source electrode two interpolar, when temperature is increased to 830 ~ 860 DEG C, keep operating air pressure 33 ~ 38Pa, under workpiece and source voltage are respectively 350 ~ 400V and 600 ~ 700V condition, start the preparation carrying out beryllium copper surface titanium alloy layer, oozing the titanium time is 1.5 ~ 2.5h;
(6) ooze after titanium terminates, be filled with ammonia, adjusting gas flow makes Ar:NH
3volume ratio be 5:3 ~ 4, air pressure is 75 ~ 90Pa, and oozing temperature is altogether 830 ~ 880 DEG C, and workpiece voltage is 600 ~ 650V, source voltage is 850 ~ 900V, after oozing 1.5 ~ 2.5h altogether, maintains normal glow discharge cooling 0.5 ~ 1h, deenergization, cuts out gas, cools to room temperature with the furnace; Obtain beryllium copper Ti+N/Ti compisite seeping layer.
3. the preparation method of beryllium copper surface according to claim 1 and 2 Ti+N/Ti compisite seeping layer, is characterized in that: the structure of described plasma surface alloying stove is as follows:
Furnace shell is cylindrical structural, in furnace shell, center is provided with workpiece negative electrode, it is negative electrode backing plate above workpiece negative electrode, beryllium copper workpiece is positioned at negative electrode backing plate center upper portion, be provided with tubular auxiliary cathode above negative electrode backing plate workpiece is placed in one, in 10cm place processing 3-φ 8mm hole above auxiliary cathode, for passing into argon gas, in 25cm place processing φ 20mm hole below auxiliary cathode, it is ammonia inlet mouth; Be provided with the Titanium board be connected with target cathode frame above beryllium copper workpiece, Titanium board is positioned at auxiliary cathode, is 15 ~ 25mm with the spacing of beryllium copper workpiece; Beryllium copper workpiece is connected with workpiece power supply, becomes workpiece pole, and Titanium board is connected with target power supply by target cathode frame, becomes source electrode; Drop-bottom perforate connects source of the gas and vacuum extractor respectively.
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| CN105734485A (en) * | 2016-04-19 | 2016-07-06 | 太原理工大学 | Preparation method of compound wear-resistant coating on surface of beryllium-copper alloy |
| CN117587357A (en) * | 2024-01-19 | 2024-02-23 | 北京开元新能科技有限公司 | Metal bipolar plate for proton exchange membrane fuel cell and preparation method and application thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105734485A (en) * | 2016-04-19 | 2016-07-06 | 太原理工大学 | Preparation method of compound wear-resistant coating on surface of beryllium-copper alloy |
| CN105734485B (en) * | 2016-04-19 | 2018-03-06 | 太原理工大学 | A kind of preparation method of beallon surface recombination wear-resistant coating |
| CN117587357A (en) * | 2024-01-19 | 2024-02-23 | 北京开元新能科技有限公司 | Metal bipolar plate for proton exchange membrane fuel cell and preparation method and application thereof |
| CN117587357B (en) * | 2024-01-19 | 2024-04-09 | 北京开元新能科技有限公司 | Metal bipolar plate for proton exchange membrane fuel cell and preparation method and application thereof |
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