CN114775003B - Electroforming liquid, electroforming method and application of electroforming liquid in laser printer fixing film - Google Patents
Electroforming liquid, electroforming method and application of electroforming liquid in laser printer fixing film Download PDFInfo
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- CN114775003B CN114775003B CN202210683004.9A CN202210683004A CN114775003B CN 114775003 B CN114775003 B CN 114775003B CN 202210683004 A CN202210683004 A CN 202210683004A CN 114775003 B CN114775003 B CN 114775003B
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/56—Electroplating: Baths therefor from solutions of alloys
- C25D3/562—Electroplating: Baths therefor from solutions of alloys containing more than 50% by weight of iron or nickel or cobalt
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D1/00—Electroforming
- C25D1/02—Tubes; Rings; Hollow bodies
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- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03G—ELECTROGRAPHY; ELECTROPHOTOGRAPHY; MAGNETOGRAPHY
- G03G15/00—Apparatus for electrographic processes using a charge pattern
- G03G15/20—Apparatus for electrographic processes using a charge pattern for fixing, e.g. by using heat
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Abstract
The invention disclosesAn electroforming liquid, an electroforming method, a product obtained by the liquid and the method and application of the product in a laser printer photographic fixing film are provided. The electroforming solution consists of nickel sulfate, nickel chloride, boric acid, cobalt sulfate, ferrous sulfate and deionized water; the pH value of the electroforming solution is 4-6. The electroforming method comprises forming a conductive path of power supply-anode-electroforming liquid-cathode-power supply, and electroforming a steel mold of cathode at 55-60 deg.C for 65 + -8 min at a current density of 2.0-4.0A/dm 2 And electrodepositing on the outer surface of the steel mould to form the nickel-iron-cobalt alloy tube blank. The electroforming solution has simple formula, easily obtained raw materials and no need of various additives; the thickness of the nickel-iron-cobalt alloy tube blank is between 30 and 60 micrometers, and the nickel-iron-cobalt alloy tube blank has excellent heat conductivity, high temperature resistance and thermal mechanical fatigue performance, and is particularly suitable for preparing a fixing film of a laser printer.
Description
Technical Field
The present invention relates to electroforming, and more particularly, to electroforming characterized by deposition of a metal material, and more particularly, to an electroforming solution, an electroforming method, a product obtained by the solution and the method, and an application thereof in a laser printer fixing film.
Background
At present, stainless steel materials are mostly used in the market for laser printer photographic fixing film alloy pipe blanks, the blanks are mostly manufactured in a multi-pass hydraulic mode, imported products are mostly adopted for the blanks, the product quality of the blanks is to be improved, and the cost is high.
The existing electroformed pipe blank products mainly have the problems of thick columnar structure, poor product strength, unstable temperature resistance, rough surface and the like. The material for the fixing film of the printer needs to meet the use requirements of high strength and high temperature resistance. The existing electroformed pipe blank cannot meet the use requirements.
Disclosure of Invention
In order to overcome the problems of thick columnar structure, poor product strength, unstable temperature resistance, rough surface and the like of the traditional electroformed pipe blank and expand the application range of the electroformed pipe blank, the invention provides a series of technical schemes as follows:
the inventors have conducted a long-term research and search and found an electrocasting solution having an excellent effect. The electroforming solution consists of nickel sulfate, nickel chloride, boric acid, cobalt sulfate, ferrous sulfate and deionized water; the pH value of the electroforming solution is 4-6.
Deionized water refers to pure water from which impurities in the form of ions have been removed. The use of tap water leaves deposits of calcium, magnesium, etc., but the use of deionized water does not present any problems.
Furthermore, the electroforming solution contains 180-220g of nickel sulfate, 6.5-8.5g of nickel chloride, 35-45g of boric acid, 3-5g of cobalt sulfate and 0.5-1.5g of ferrous sulfate per liter of deionized water.
Preferably, the electroforming solution formulation contains 193-209g of nickel sulfate, 7g of nickel chloride, 39-41g of boric acid, 3.7-4.1g of cobalt sulfate and 0.8-1.1g of ferrous sulfate per liter of deionized water.
The existing electroformed pipe blank products mostly adopt electroformed pure nickel, and have the defects that the strength is lost at the temperature of more than 280 ℃, serious brittle fracture occurs, and the existing electroformed pipe blank products cannot be used at all. The electroforming solution contains ferrous sulfate to avoid brittle fracture after heating, but the ferrous sulfate with improper proportioning can generate a large amount of pinholes in a casting layer. The obtained tube blank product has certain resilience at high temperature, but the thermomechanical property is still poor. Thus, the electrocasting solution of the present invention strictly limits the amount of ferrous sulfate added, and is prepared by adding 0.5 to 1.5g of ferrous sulfate, preferably 0.8 to 1.1g of ferrous sulfate, to one liter of deionized water.
The cobalt sulfate contained in the electroforming solution can improve the wear resistance of the tube blank. The electroforming solution of the invention is prepared by adding 3-5g of cobalt sulfate, preferably 3.7-4.1g of cobalt sulfate into one liter of deionized water.
In a word, one of the technical keys of the invention is to strictly limit the contents of nickel, iron and cobalt in the electroforming solution, otherwise, qualified nickel-iron-cobalt alloy tube blank products cannot be produced.
The invention also provides an electroforming method, which adopts the electroforming liquid.
Further, the electroforming method is to form a power source-anode-electroforming liquid-cathode-power sourceA conductive path for electroforming the steel mold of the cathode for 65 +/-8 min, wherein the electroforming solution has a temperature of 55-60 ℃ and a current density of 2.0-4.0A/dm 2 And electrodepositing on the outer surface of the steel die to form the nickel-iron-cobalt alloy tube blank.
Furthermore, the power supply is a digital pulse power supply. That is, in the present invention, a dc power supply is not used. The digital pulse power supply can adopt TLM-24/1000CVC type, TLM-300/100 type, SMD-300 type and other professional equipment power supplies. These power sources are readily available on the market.
Furthermore, the anode is a nickel plate.
Furthermore, the steel mould is arranged at the position of a double-tip of demoulding equipment and is fixed through a sliding module; and after the treatment of the demoulding pressure head above, taking down the nickel-iron-cobalt alloy pipe blank from the steel mould. The step solves the problem that the electroforming pipe blank tightly coats the die, so that the die cannot be removed. Therefore, the steel die can be repeatedly put into production, and the production efficiency is improved.
The cathode of the invention is a steel die, a cylindrical die is adopted as a forming die, the forming die is generally made of chrome-plated bearing steel, the diameter of the die is generally 18 +/-0.005 mm, 24 +/-0.005 mm, 30 +/-0.005 mm, 47 +/-0.005 mm, 80 +/-0.005 mm and the like, and the length of the die is generally 300 plus or minus 500 mm.
The invention also provides a nickel-iron-cobalt alloy tube blank which is prepared by the electroforming method. The nickel-iron-cobalt alloy tube blank can be applied to the preparation of a laser printer fixing film.
Further, spraying one or more of polytetrafluoroethylene, fluorinated ethylene propylene and tetrafluoroethylene-perfluoroalkoxy vinyl ether copolymer on the outer surface of the nickel-iron-cobalt alloy pipe blank to obtain the laser printer fixing film.
Finally, the invention also provides a manufacturing method of the nickel alloy tube blank for the fixing film of the laser printer, which adopts the electroforming solution and is manufactured by the electroforming method.
The invention has the beneficial effects that:
firstly, the formula of the electroforming solution is simple, the raw materials are easy to obtain, and various additives are not needed.
Secondly, the electroforming method can accurately control the thickness of the tube blank, and the thickness of the obtained nickel-iron-cobalt alloy tube blank is quite thin and is between 30 and 60 micrometers.
And thirdly, the nickel-iron-cobalt alloy tube blank has excellent heat conductivity, high temperature resistance and thermal mechanical fatigue performance, and is particularly suitable for preparing a fixing film of a laser printer.
Drawings
FIG. 1 is a schematic front view of an electrocasting apparatus of the present invention.
FIG. 2 is a schematic top view of an electroforming apparatus of the present invention.
FIG. 3 is a schematic view of the demolding apparatus of the present invention.
Description of reference numerals: 1-steel mould; 2, a transmission gear; 3-rotating the conductive column; 4-digital pulse power supply; 5-anode nickel plate; 6-an electroforming pool; 7-electroforming solution; 8, a circulating pump; 9-rotating the motor;
11-double apex position; 12-a slide module; 13-demolding press head.
Detailed Description
Example 1
Preparing 200 liters of deionized water, and adding 200g of nickel sulfate, 7g of nickel chloride, 40g of boric acid, 4g of cobalt sulfate and 1g of ferrous sulfate into each liter of deionized water to prepare an electroforming solution; the pH of the electrocasting solution was 5.
Example 2
Preparing an electroforming solution by adding 193g of nickel sulfate, 7g of nickel chloride, 39g of boric acid, 3.7g of cobalt sulfate and 0.8g of ferrous sulfate into 200 liters of deionized water per liter of deionized water; the pH of the electrocasting solution was 6.
Example 3
Preparing 200 liters of deionized water, and adding 209g of nickel sulfate, 7g of nickel chloride, 41g of boric acid, 4.1g of cobalt sulfate and 1.1g of ferrous sulfate into each liter of deionized water to prepare an electroforming solution; the pH of the electrocasting solution was 4.
Example 4
As shown in fig. 1 to 3, a cylindrical bearing steel mold 1 is subjected to surface cleaning treatment to remove surface oil stains and floating dust, and then is assembled below a transmission gear 2 to serve as a negative stage. One section of the die 1 is fixedly connected with the transmission gear 2 through a screw rod, a rotary conductive column 3 is fixed above the transmission gear 2, and the rotary conductive column 3 is connected with the cathode end of the digital pulse power supply 4. An anode nickel plate 5 is fixed on the electroforming pool 6 and is connected with the anode end of the digital pulse power supply 4. The electroforming bath 6 is filled with the electroforming solution 7 as described in example 1, and the liquid surface completely covers the mold 1 and the anode nickel plate 5. The temperature of the electroforming solution was 55 ℃.
And starting the electroforming liquid circulating pump 8, and uniformly flushing the die 1 by the electroforming liquid 7 through a circulating pipeline, so as to form a conductive path of the power supply 4-the anode 5-the electroforming liquid 7-the cathode 1-the power supply 4.
The digital pulse power supply 4 is started, and the rotating motor 9 is started. The current density is 3.3A/dm 2 . After 60 minutes of treatment, a cylindrical nickel-iron-cobalt alloy tube blank with the inner diameter of 18mm and the length of 300mm is formed on the outer surface of the bearing steel die 1 through electrodeposition. The thickness of the tube blank was 33 microns.
Mounting the bearing steel die 1 to a double-tip position 11 of a demolding device, and fixing the bearing steel die through a sliding module 12; and after the treatment by the upper demoulding pressure head 13, taking the nickel-iron-cobalt alloy tube blank off the bearing steel mould 1.
Example 5
Example 5 was substantially the same as example 4 except that the electrocasting solution of example 2 was used, the electrocasting solution having a temperature of 60 ℃ and a current density of 3.3A/dm 2 . After the treatment for 60 minutes, a cylindrical nickel-iron-cobalt alloy tube blank with the inner diameter of 30mm and the length of 300mm is formed on the outer surface of the bearing steel die 1 through electrodeposition. The thickness of the tube blank was 40 microns.
Example 6
Example 6 is substantially the same as example 4 except that the electrocasting solution of example 3 is used. After 60 minutes of treatment, a cylindrical nickel-iron-cobalt alloy tube blank with the inner diameter of 24mm and the length of 450mm is formed on the outer surface of the bearing steel die 1 through electrodeposition. The thickness of the tube blank was 40 microns.
Comparative example 1
Preparing nickel-containing electroforming solution, wherein the nickel-containing electroforming solution mainly comprises nickel sulfate, nickel chloride, boric acid, sodium chloride, water and a conventional additive, adjusting the pH value of the casting solution to be 3.0, operating by adopting a single-use die through a roll casting process, and then damaging the die to obtain a pure nickel pipe blank made of nickel.
Comparative example 2
Preparing nickel-iron-containing cast solution, which mainly comprises nickel sulfate, nickel chloride, boric acid, ferrous sulfate, sodium chloride, water and two conventional additives, adjusting the pH value of the cast solution to 3.3, and then operating by adopting a hang-casting process to obtain an alloy pipe blank made of nickel iron.
TABLE 1 Heat conductivity of the tube blanks
| Sample (I) | Example 4 | EXAMPLE 5 | EXAMPLE 6 | Comparative example 1 | Comparative example 2 | Round 316# stainless steel tube with wall thickness of 40 microns and diameter of 30mm |
| Thermal conductivity, W/m, seed and K | 1.45 | 1.46 | 1.47 | 1.43 | 1.45 | 0.65 |
TABLE 2 high temperature resistance of the tube blank (plastic deformation after external force is applied, characterized by minor axis length and its rate of change)
The high temperature resistance test method comprises the following steps:
the method is characterized by the change of out-of-roundness of the tube blank before and after heat resistance and under the condition of applying external force.
(1) Pretreatment: cleaning the surface of the metal pipe blank, vertically placing the metal pipe blank in a high-temperature blast drying oven, heating to 400 ℃ within about 1 hour, keeping the temperature for 30min, closing the drying oven, heating, and naturally cooling to below 50 ℃ and taking out.
(2) Horizontally placing the pretreated pipe blank on a plane, applying pressure from the upper part to deform the pipe blank into an elliptical section, limiting the minor axis of the elliptical section to be 60 percent of the nominal diameter, and releasing pressure after keeping for 24 hours; and left to stand for 10min, 60min and 120min, and the dimensional change of the short axis (i.e. the height of the round tube in the pressed direction) of the sample is measured.
Example 7
Taking the nickel-iron-cobalt alloy tube blank obtained in the embodiment 4 as a base material tube blank, spraying polytetrafluoroethylene on the surface of the base material tube blank to serve as a bottom coating, spraying fluorinated ethylene propylene to serve as a top coating, baking at 385 ℃ for 15min, and cutting to obtain the laser printer fixing film.
Example 8
The nickel-iron-cobalt alloy tube blank obtained in example 5 was used as a base material tube blank, a tetrafluoroethylene-perfluoroalkoxy vinyl ether copolymer was sprayed on the surface of the base material tube blank as a topcoat, and after baking at 375 ℃ for 15min, a laser printer fixing film was obtained after cutting.
Example 9
The nickel-iron-cobalt alloy tube blank obtained in example 6 was used as a base material tube blank, a tetrafluoroethylene-perfluoroalkoxy vinyl ether copolymer was sprayed on the surface of the base material tube blank as a topcoat, and after baking at 375 ℃ for 20min, a laser printer fixing film was obtained after cutting.
Comparative example 3
The pure nickel pipe blank obtained in the comparative example 1 was used as a base material pipe blank, a tetrafluoroethylene-perfluoroalkoxy vinyl ether copolymer was sprayed on the surface of the base material pipe blank as a top coat, and after baking at 375 ℃ for 20min, a laser printer fixing film was obtained after cutting.
Comparative example 4
Taking the ferronickel alloy pipe blank obtained in the comparative example 2 as a base material pipe blank, spraying tetrafluoroethylene-perfluoroalkoxy vinyl ether copolymer as a surface coating on the surface of the base material pipe blank, baking at 375 ℃ for 20min, and cutting to obtain the laser printer fixing film.
The testing method of the thermomechanical fatigue property comprises the following steps:
and (3) observing the degree of appearance and quality change of the tube blank before and after the test by using a laser printer as a test instrument to evaluate the performance.
When the laser printer works, the heater in the fixing film can heat the metal pipe blank to the high temperature of 220-250 ℃, and under the action of a series of mechanical structures, the fixing film rotates around the heating core at the speed of about 2.2-3 rpm; in this test, the number of printed sheets of a4 paper was used to represent the time of thermal mechanical fatigue. The fixing film is externally pressed and rubbed by elastic heat-resistant rubber, the inside of the fixing film is supported by a plane (heating sheet) in a narrow and long strip shape, and the inner surface of the fixing film is in sliding fit with the supporting heating sheet.
(1) Sample preparation: cleaning the surface of a metal tube blank, coating a composite coating consisting of PI and PTFE emulsion as a base coating, wherein the thickness of a dry film is 3-10 mu m, and drying at 120-180 ℃ for 10-30 min; and then coating a PTFT anti-sticking coating, wherein the thickness of a dry film is 5-20 mu m, and sintering for 30min at 400 ℃ to successfully prepare a complete fixing film.
(2) Measurement:
according to the test method of the operation test and the service life test in the mechanical industry standard JB/T13030-2017 resin-based fixed film technical conditions for xerography (printing and multifunctional) equipment, the original fixed film on the printer is replaced by the sample, and the printer is started to operate. And recording. The recording data includes the following:
firstly, the roundness, the quality, the length, the appearance and the like of a fixation film sample before testing; the following swatches were printed in order for comparison: a. a full image (including at least full black) C of the printed proof sheet before the fixing film is not replaced; b. replacement sample original proof S0; then, when the blank paper (a 4) 1000, 2000, 5000, 10000, 20000, 30000, 40000, 50000, 60000, 70000, 80000, 90000, 100000 pages are fed again, a proof sheet is printed, S1000, S2000, S5000, S10000, S20000, S30000, S40000, ·; and the sample fixation film appearance, length, mass change were recorded.
The fixation firmness is a main index related to the neutralization and fixation of the quality of a printed product; in the case where other conditions are not changed, only the fixing film is replaced, and if the fixing fastness is changed, the performance of the fixing film can be objectively evaluated. The inventors followed the test method of section 7.12 (regarding fixing fastness) in the GB/T10073-2021 xerographic print image quality evaluation method, namely:
a. a sheet obtained by cutting a plate specified in GB/T4591 into a width of 30 mm. + -. l mm with respect to a solid circle (A3 horizontal direction and A4 vertical direction) at the center on each copy was used as a sample, and the density value D of the solid circle was measured by a reflection densitometer before ；
b. Placing the sample on a friction tester, placing the test point at the center of the friction table, rubbing twice, and measuring the reflection density value D after ；
c. The fixation fastness was calculated as follows.
D fix = D after / D before × 100%
In the formula:
D fix -fixing fastness;
D afIer -density value of solid circle after rubbing;
D before -density value of solid circle before rubbing.
The fixing film continuously rubs with plugs on two sides in rotation, so that two ends of the fixing film are abraded; if the fixation film is tempered at high temperature, the two ends of the fixation film are abraded more, and the metal pipe blank is shortened;
when the fixing film works, the fixing film rubs with the heating sheet ceramic, if the strength is poor, some metal powder can be ground, lubricating grease is thickened and dried, and the paper jam phenomenon can occur. When the paper jam occurs for the first time, after removing the reasons of other parts of the equipment, the sample fixing film is detached, the sample fixing film is installed again after cleaning the inner wall (proper high temperature resistant grease can be added), if the paper jam occurs again due to the reasons of the fixing film, the test is stopped, and various data are recorded.
Table 3 example 7 print performance and example 4 thermo-mechanical fatigue test (test using hp laserjet P1505 printer)
Table 4 example 8 print performance and example 5 thermo-mechanical fatigue test (test using hewlett packard laserjet 4300 printer)
Table 5 example 9 print performance and example 6 thermo-mechanical fatigue test (test using hewlett packard laserjet4700 printer)
TABLE 6 comparative example 3 print performance and comparative example 1 thermo-mechanical fatigue test (test using Hewlett packard Laserjet P1505 printer)
TABLE 7 comparative example 4 print performance and comparative example 2 thermo-mechanical fatigue test (test using Hewlett packard Laserjet P1505 printer)
Through the tests, the product prepared by the formula and the process has obvious improvement on heat resistance and thermal mechanical fatigue, and can meet the requirement of serving as a fixing film tube blank of a printer.
The present invention relates to an electroforming solution, an electroforming method and an application thereof in a fixing film of a laser printer, and the principle and the implementation mode of the present invention are explained by applying specific examples, and the description of the above examples is only used for helping to understand the scheme and the core idea of the present invention. It should be noted that the present invention is not limited to the above-described exemplary embodiments, and those skilled in the art can make various changes and modifications without departing from the scope or spirit of the present invention. Meanwhile, for a person skilled in the art, according to the idea of the present invention, the specific implementation and the application range may be changed; accordingly, in view of the above, this summary should not be construed as limiting the invention.
Claims (10)
1. An electroforming solution consists of nickel sulfate, nickel chloride, boric acid, cobalt sulfate, ferrous sulfate and deionized water; the nickel-cobalt-based catalyst is characterized in that each liter of deionized water contains 193-209g of nickel sulfate, 7g of nickel chloride, 39-41g of boric acid, 3.7-4.1g of cobalt sulfate and 0.8-1.1g of ferrous sulfate; the pH value of the electroforming solution is 4-6.
2. The electroforming solution according to claim 1, wherein the deionized water contains 200g of nickel sulfate, 7g of nickel chloride, 40g of boric acid, 4g of cobalt sulfate and 1g of ferrous sulfate per liter; the pH of the electroforming solution was 5.
3. An electrocasting method using the electrocasting solution according to any one of claims 1 to 2.
4. According to claim 3The electroforming method forms a power supply-anode-electroforming liquid-cathode-power supply conductive path, and carries out electroforming treatment on a steel mould of a cathode, and is characterized in that the treatment time is 65 +/-8 minutes, the temperature of the electroforming liquid is 55-60 ℃, and the current density is 2.0-4.0A/dm 2 And electrodepositing on the outer surface of the steel mould to form the nickel-iron-cobalt alloy tube blank.
5. The electroforming method according to claim 4, wherein the power supply is a digital pulse power supply.
6. The electroforming method according to claim 4, wherein the anode is a nickel plate.
7. The electroforming method according to claim 4, wherein the steel mold is mounted to a double tip position of a demolding apparatus, and fixed by a slide module; and after the treatment by the upper demoulding pressure head, taking the nickel-iron-cobalt alloy tube blank down from the steel mould.
8. A nickel-iron-cobalt alloy shell produced by the electroforming method according to any one of claims 3 to 7.
9. Use of a nickel iron cobalt alloy tubestock as claimed in claim 8 in the manufacture of a laser printer fuser film.
10. A method of manufacturing a nickel alloy shell for a fixing film of a laser printer, characterized in that the electrocasting method according to any one of claims 3 to 7 is employed.
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| JP4532290B2 (en) * | 2005-01-11 | 2010-08-25 | キヤノン電子株式会社 | Fixing belt and image forming apparatus |
| CN101872147A (en) * | 2009-04-22 | 2010-10-27 | 庞力 | Reinforced thin-wall metal base pipe and manufacturing method thereof |
| CN103205604B (en) * | 2012-01-16 | 2016-08-10 | 昆山允升吉光电科技有限公司 | A kind of preparation method of dilval |
| CN103205630B (en) * | 2012-01-16 | 2016-04-27 | 昆山允升吉光电科技有限公司 | A kind of Ferro-nickel alloy material and preparation method thereof |
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| 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 |
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