Method for preparing bronze etching material
The method of preparing bronze etching materials through multiple staged annealing and tempering solves the warping and deformation problem of large-size bronze etching materials, and realizes rapid prototyping and low warping etching materials, which are suitable for new energy vehicles, rail transportation, aerospace, smart medical and electrical power fields.
Patent Information
- Application Number
- CN202211605724.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2022-12-14
- Publication Date
- 2026-01-02
- Estimated Expiration
- 2042-12-14
AI Technical Summary
Existing bronze etching materials cannot simultaneously meet the requirements of flatness and minimal internal residual stress when processing large sizes, resulting in warping and high costs, making it difficult to achieve large-scale production.
Bronze etching blanks are used, and bronze etching materials are prepared by multiple staged annealing and tempering processes, combined with appropriate machining rates. This avoids the strip processing stress caused by using large machining rates and achieves rapid forming.
It achieves rapid prototyping and dimensional stability of bronze etching materials, reduces production costs, is suitable for industrial-scale production, has a warpage of less than 3mm, and increases the yield strength ratio by more than 10%.
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Figure CN116837308B_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of metal material production processes, and in particular to a method for preparing bronze etching materials. Background Technology
[0002] Bronze is an ancient alloy material that continues to shine in industries that have a significant impact on national economy and people's livelihood, such as new energy vehicles, rail transportation, aerospace, smart healthcare, and electrical power. For example, in the patent application number 202111388804.X, entitled "A method for preparing a low-plate type I-value tin-phosphorus bronze strip", bronze material is used as a heat sink material for smartphones.
[0003] Bronze materials used in semiconductor chip manufacturing generally fall into two categories: stamping materials for stamping production and etching materials for engraving using chemical agents. Stamping materials are primarily made from bronze, processed through casting, rolling, annealing, and straightening. The aforementioned heat spreader material is an example of a stamping material produced using this process. Etching materials, on the other hand, require etchability and need to produce clear and stable etching.
[0004] However, practical production experience shows that using etching materials with a width of 200-300mm or more makes it difficult to simultaneously meet etching process requirements such as flatness, minimal internal residual stress, and no significant warping after etching. To achieve high flatness during production, the processing rate cannot be too low; however, a high processing rate leads to high residual stress within the material, making it prone to warping and deformation after etching, resulting in batch scrap. Therefore, producing large-size etching bronze materials is difficult, costly, and unsuitable for large-scale production. Summary of the Invention
[0005] Therefore, it is necessary to provide a method for preparing bronze etching materials to address at least one of the problems mentioned above.
[0006] The method for preparing bronze etching material provided in this invention application includes the following steps:
[0007] Prepare bronze etching blanks, and homogenize and anneal the bronze etching blanks to obtain bronze etching blanks for use;
[0008] The bronze etching blank to be used is rough rolled to a first predetermined thickness and the edges are trimmed. Then, it is annealed to obtain the first blank.
[0009] The first billet is subjected to a first precision rolling and a first tempering to obtain a second billet;
[0010] The second billet is subjected to a second finishing roll and a second tempering to obtain a third billet, wherein the processing rate of the second finishing roll is 30% to 35%.
[0011] carrying out third finish rolling and third tempering on the third blank to obtain a fourth blank, a processing rate of the third finish rolling being 10.0-12.5%;
[0012] carrying out fourth finish rolling and fourth tempering on the fourth blank to obtain a first finished product, a processing rate of the fourth finish rolling being 10.0-15.5%;
[0013] after cleaning and passivating the first finished product, obtaining a bronze etching strip.
[0014] In one of the embodiments, the step of preparing the bronze etching blank comprises:
[0015] roasting the oil-containing and / or water-containing bronze scrap, melting the bronze scrap together with tin ingots into qualified copper water in a furnace, and after standing for 3-5 minutes, transferring the copper water into a holding furnace for holding;
[0016] casting the copper water after standing into an electromagnetic casting crystallizer to obtain the bronze etching blank.
[0017] In one of the embodiments, the step of melting the bronze scrap together with tin ingots into qualified copper water has a melting temperature of 1200-1300℃.
[0018] In one of the embodiments, the step of standing for 3-5 minutes and then transferring into a holding furnace for holding has a holding temperature of 1190-1230℃.
[0019] In one of the embodiments, the step of casting the copper water after standing into an electromagnetic casting crystallizer has an electromagnetic frequency of the electromagnetic casting crystallizer of 20-25Hz, and the temperature of the drawn blank is 360-450℃.
[0020] In one of the embodiments, the step of roughing and breaking down the bronze etching blank after milling the bronze etching blank comprises homogenizing annealing the bronze etching blank, and the annealing temperature is 300 / 650-700℃, and the holding time of the annealing is 8-10 hours.
[0021] In one of the embodiments, the annealing temperature of the softening annealing is 280 / 450-550℃, and in the step of obtaining the first blank after the subsequent annealing treatment, the annealing temperature is 650 / 700℃.
[0022] In one of the embodiments, the step of carrying out first finish rolling and first tempering on the first blank has a first tempering temperature of 650-700℃.
[0023] In the step of carrying out second finish rolling and second tempering on the second blank, the second tempering has a tempering temperature of 400-500℃.
[0024] In one of the embodiments, the third annealing temperature of the third annealing in the step of performing third finish rolling and third annealing on the third blank is 350-450 DEG C.
[0025] The fourth annealing temperature of the fourth annealing in the step of performing fourth finish rolling and fourth annealing on the fourth blank is 230-300 DEG C.
[0026] In one of the embodiments, the step of cleaning and passivating the first finished product comprises: cleaning the first finished product, and cleaning with sulfuric acid, the concentration of the sulfuric acid being 10.0-15.0%.
[0027] The technical solutions provided in the embodiments of the present application have the following beneficial technical effects:
[0028] The preparation method of bronze etching material provided by the present application adopts bronze etching blank, the blank is subjected to multiple sectional annealing and multiple annealing, and appropriate multiple rolling is performed between the annealing, orderly rolling is performed with the processing rate distributed in steps, the continuous use of large processing rate is avoided to reduce the processing stress of the strip and is not conducive to etching, the rapid forming of bronze etching material can be realized, and the industrialized mass production can be performed.
[0029] Additional aspects and advantages of the present application will be described in subsequent sections, and will be understood in detail from the subsequent description, or by understanding the specific implementation of the present application. BRIEF DESCRIPTION OF DRAWINGS
[0030] Figure 1 The figure is a flowchart of the preparation method of bronze etching material in one embodiment of the present application.
[0031] Figure 2 The figure is a process flowchart of bronze etching strip material in one embodiment of the present application. DETAILED DESCRIPTION
[0032] In order to facilitate the understanding of the present application, the present application will be described more fully below with reference to the related drawings. The drawings show possible embodiments of the present application. However, the present application can be realized in many different forms, and is not limited to the embodiments described herein by means of the drawings. The embodiments described by reference to the drawings are exemplary, and are used to make the understanding of the disclosure of the present application more thorough and comprehensive, and cannot be interpreted as a limitation of the present application. In addition, if detailed description of known technology is not necessary for the features of the present application shown, these technical details can be omitted.
[0033] Those skilled in the art will appreciate that unless otherwise defined, all terminology used herein, including technical and scientific terms, has the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. It will be further understood that terms, such as those defined in commonly used dictionaries, should be interpreted as having a meaning that is consistent with their meaning in the context of the relevant art and will not be interpreted in an idealized or overly formal sense unless expressly so defined herein.
[0034] Those skilled in the art will appreciate that unless otherwise stated, the singular forms "a," "an," and "the" include plural referents. It will be further understood that the terms "comprises" and / or "comprising," as used herein, specify the presence of stated features, integers, steps, operations, elements, and / or components, but do not preclude the presence or addition of one or more other features, integers, steps, operations, elements, components, and / or groups thereof. It will be understood that the terms "and / or," "and / or," as used herein, encompass all of the possible combinations of one or more of the associated listed items and that the term "and / or" is used in its full sense, i.e., "and / or" is used in its conjunctive sense as well as in its disjunctive sense.
[0035] The technical solutions of the present application and how the technical solutions solve the above technical problems will be described in detail below with specific examples.
[0036] The present application provides a preparation method of bronze etching material, as shown in the formula: Figure 1 The preparation method comprises the following steps:
[0037] S100: preparing bronze etching blank, homogenizing annealing the bronze etching blank to obtain bronze etching blank for use. Optionally, the step of preparing bronze etching blank comprises: baking oil-containing and / or water-containing bronze scrap, melting the bronze scrap together with tin ingot into copper water with qualified composition in a furnace, and then transferring the copper water into a holding furnace for holding after standing for 3-5 minutes; pouring the standing copper water into an electromagnetic casting crystallizer to produce bronze etching blank. In the copper water with qualified composition, Sn is 4.5-6.5%, P is 0.09-0.10%, Pb is 0.01-0.015%, Ni is 0.02-0.05%, Zn is 0.01-0.05%, and Cu+Sn+Pmin is 99.8%. In the step of melting the bronze scrap together with tin ingot into copper water with qualified composition, the melting temperature is 1200-1300°C. In the step of transferring the copper water into a holding furnace for holding after standing for 3-5 minutes, the holding temperature is 1190-1230°C. In the step of pouring the standing copper water into an electromagnetic casting crystallizer, the electromagnetic frequency of the electromagnetic casting crystallizer is 20-25 Hz, and the temperature of the drawn blank is 360-450°C.
[0038] S200: rough rolling and opening of the bronze etching blank, rolling to a first predetermined thickness and cutting edges, and then annealing to obtain a first blank. Optionally, in the step of rough rolling and opening of the bronze etching blank after milling of the bronze etching blank, the bronze etching blank is subjected to homogenizing annealing, the annealing temperature is 300 / 650-700℃, the annealing time is 8-10 hours. Then the annealing temperature is 280 / 450-550℃; in the step of annealing to obtain the first blank, the annealing temperature is 650 / 700℃.
[0039] S300: first finish rolling and first tempering of the first blank to obtain a second blank. The first tempering temperature is 650-700℃, and the first finish rolling processing rate is 60%-70%.
[0040] S400: second finish rolling and second tempering of the second blank to obtain a third blank, the second finish rolling processing rate is 30%-35%. The second tempering temperature is 400-500℃.
[0041] S500: third finish rolling and third tempering of the third blank to obtain a fourth blank, the third finish rolling processing rate is 10.0-12.5%. The third tempering temperature is 350-450℃.
[0042] S600: fourth finish rolling and fourth tempering of the fourth blank to obtain a first finished product, the fourth finish rolling processing rate is 10.0-15.5%. The fourth tempering temperature is 230-300℃.
[0043] S700: cleaning and passivating the first finished product to obtain a bronze etching strip.
[0044] The preparation method of the bronze etching material provided by the application uses a bronze etching blank, the blank is subjected to multiple segment annealing and multiple tempering, and appropriate multiple rolling is performed between the annealing to orderly roll with a ladder distribution of processing rates, so that the continuous use of a large processing rate is avoided, the processing stress of the strip is large and is not conducive to etching, the rapid forming of the bronze etching material can be realized, and industrialized mass production can be carried out.
[0045] Optionally, in an embodiment of the application, the step of cleaning and passivating the first finished product comprises: cleaning the first finished product, and using sulfuric acid for cleaning, the concentration of the sulfuric acid is 10.0-15.0%. The concentration of the passivation solution is 0.1-0.15%.
[0046] The application adopts bronze electromagnetic casting billet, the billet is subjected to secondary segmented annealing, secondary high-temperature tempering, secondary medium-temperature tempering, primary low-temperature tempering, annealing and rolling with appropriate processing rate, to form the best etching material preparation method for eliminating etching stress (specifically eliminating processing stress at 300 / 650-700℃, 280 / 450-550℃, 650-700℃, 400-500℃, 350-450℃, 230-300℃), which can effectively prepare the etching strip from the bronze billet, so that it becomes the strip which is more than 10% higher than the ordinary bronze material with the yield ratio of 0.7-0.85, and in the process of etching the 30*300mm plate, the warping height is less than 3mm, the warping degree of the ordinary bronze material after etching reaches 30mm, and the bronze etching material prepared by the preparation method provided by the application can keep the size of the etching product stable and regular.
[0047] In the preparation method of the application, the intermediate billet is rolled to the etching material finished product by using two small processing rates of 10.0-12.5% / 10-15.5%, which avoids using a large processing rate, so that the processing stress of the strip is large and is not conducive to etching, is conducive to rapid forming, and can also reduce the new stress generated by multiple drawing and forming.
[0048] The following is a specific embodiment:
[0049] As shown in Figure 2 , the whole process of preparing the bronze etching material in the embodiment is as follows:
[0050] 1) Preparation of bronze etching billet:
[0051] ① Classify the bronze old material, bake the oil and water containing material to 180-250℃, pack the scrap material, and the block weight is 100-300kg; cut the tin ingot into blocks for standby.
[0052] ② Add the scrap material and block material to the furnace in turn; heat and melt to 1300℃; take a sample to measure the composition, mill the surface to a depth of 10mm, and add tin blocks as needed; after the composition is qualified, stand for 3-5 minutes.
[0053] ③ Transfer the copper water with a weight of 800-1000kg to the holding furnace; the holding temperature is 1190-1230℃.
[0054] ④ Cast the billet by electromagnetic casting crystallizer with a specification of 650*16, electromagnetic frequency of 20-25HZ; the strip billet is drawn out at a temperature of 360-450℃; the standby bronze etching billet weighs 9500kg.
[0055] 2) Preparation of bronze etching strip:
[0056] ① Homogenize and anneal the bronze blank to be etched at 300 / 650~700℃ for 8-10 hours. The homogenization annealing is divided into two stages. In the first stage, heat to 300 degrees Celsius and hold for a period of time, then heat to 650~700℃ and continue to hold.
[0057] ② After milling the 16mm (standard thickness) billet by 4% to 7.5%, rough roll it to 2.50mm (optimal thickness); after softening annealing at 280 / 450 to 550℃, roll it to 2% to 3% of the 0.80mm trim width; anneal the 0.80mm billet in a vertical furnace at 650 / 700℃. This yields a first billet with a thickness of 0.8mm.
[0058] ③ The first billet is precision rolled to a minimum thickness of 0.40-0.50 mm (the second billet after the first precision rolling); then tempered at 650-700℃.
[0059] ④ The blank thickness is finished rolled to a minimum blank thickness of 0.28-0.35 mm, and the processing rate (processing rate = (incoming thickness - rolled thickness) / incoming thickness * 100%) is controlled at 30.0-35.0%; then it is tempered at a medium temperature of 400-500℃ to obtain the third billet.
[0060] ⑤ The blank thickness is finished rolled to a secondary blank thickness of 0.25-0.30 mm, and the processing rate is controlled at 10.0-12.5%; then it is tempered at 350-450℃ to obtain the fourth blank.
[0061] ⑥ The remaining thickness is precision rolled to a finished thickness of 0.20-0.25 mm, with the processing rate controlled at 10.0-15.5%; then tempered at a low temperature of 230-300℃ to obtain the first finished product.
[0062] ⑦ Clean the first finished product, namely the 0.20-0.25mm bronze etched strip; control the sulfuric acid concentration at 10.0-15.0%; and the passivation concentration at 0.1-0.15%.
[0063] 3) Post-processing of products:
[0064] The strip is cut using a vacuum roller slitting machine. The unwinding tension is 0.32KN, and the winding tension is 2KN. The vacuum roller pressure is -117mbar / -51%, the vacuum plate position is 760mm, and the cutter diameter is 240-250mm. The 620mm master strip is slit into 200-300mm strips and placed on the cross arm. The bronze etching material is packaged into the product using vertical wooden plywood.
[0065] The bronze etching material prepared by the method has a measured compressive strength of 615 MPa, a yield strength greater than 560 MPa, a hardness of HV190-200, an elongation greater than 20%, an electrical conductivity of 15.73 S / m, a bending resistance of 90 degrees R / T = 1, no cracking, a 300 / 30 mm etching stress test warpage of less than 10 mm, and can be widely used in new energy vehicles, rail transit, aerospace, medical treatment, power, military and civilian, and the like.
[0066] Those skilled in the art can understand that the steps, measures and schemes in various operations, methods and processes discussed in the present application can be alternated, changed, combined or deleted. Further, other steps, measures and schemes in various operations, methods and processes discussed in the present application can also be alternated, changed, rearranged, decomposed, combined or deleted. Further, the steps, measures and schemes in various operations, methods and processes in the prior art can also be alternated, changed, rearranged, decomposed, combined or deleted.
[0067] The terms "first", "second" are only for descriptive purpose, and cannot be understood as indicating or implying relative importance or implicitly indicating the number of the indicated technical features. Therefore, the features defined with "first", "second" can explicitly or implicitly include one or more of the features. In the description of the present application, the meaning of "a plurality of" is two or more, unless otherwise specified and limited.
[0068] In the description of the present application, it should be noted that, unless otherwise explicitly specified and limited, the terms "mounting", "connecting", "connection" should be understood in a broad sense, for example, can be fixed connection, can also be detachable connection, or integrally connected; can be directly connected, or indirectly connected through an intermediate medium; can be the communication inside two elements. For those skilled in the art, the specific meaning of the above terms in the present application can be understood according to the specific circumstances.
[0069] In the description of the present application, specific features, structures, materials or characteristics can be combined in any one or more embodiments or examples in a suitable manner.
[0070] It should be understood that although the steps in the flowcharts of the drawings are shown in a sequential order following the arrows, the steps are not necessarily executed in the order indicated by the arrows. Unless explicitly stated otherwise herein, the execution of the steps is not strictly limited to the order indicated by the arrows, and can be executed in other orders. Moreover, at least some of the steps in the flowcharts of the drawings can include multiple sub-steps or multiple stages, which are not necessarily executed at the same time, but can be executed at different times, and the execution order of which is not necessarily sequential, but can be round-robin or alternating with at least some of the other steps or sub-steps or stages of other steps.
[0071] The above only describes some embodiments of the present application, and it should be pointed out that for those skilled in the art, without departing from the principles of the present application, a number of improvements and refinements can be made, which should also be considered as the protection scope of the present application.
Claims
1. A method for preparing a bronze etching material, characterized by, Includes the following steps: The preparation of bronze etching blanks includes: baking oily and / or watery old bronze materials, melting them together with tin ingots in a furnace to obtain copper of qualified composition, letting them stand for 3-5 minutes and then transferring them to a holding furnace for holding; casting the copper after standing into an electromagnetic casting crystallizer to produce bronze etching blanks; and performing homogenization annealing on the bronze etching blanks to obtain bronze etching blanks ready for use. The bronze etching blank to be used is rough rolled to a first predetermined thickness and the edges are trimmed. Then, it is annealed to obtain the first blank. The first billet is subjected to a first precision rolling and a first tempering to obtain a second billet; The second billet is subjected to a second finishing roll and a second tempering to obtain a third billet, wherein the processing rate of the second finishing roll is 30% to 35%. The third billet is subjected to a third finishing roll and a third tempering to obtain a fourth billet, wherein the processing rate of the third finishing roll is 10.0 to 12.5%. The fourth billet is subjected to a fourth finishing roll and a fourth tempering to obtain the first finished product, wherein the processing rate of the fourth finishing roll is 10.0 to 15.5%. After cleaning and passivating the first finished product, bronze etched strip is obtained.
2. The method for preparing a bronze etching material according to claim 1, characterized by, In the step of melting the copper ingots together with tin ingots in a furnace to produce molten copper of acceptable composition, the melting temperature is 1200-1300℃.
3. The method for preparing bronze etching material according to claim 1, characterized in that, In the step of letting it stand for 3 to 5 minutes and then transferring it to the heat preservation furnace, the heat preservation temperature is 1190 to 1230℃.
4. The method of preparing a bronze etching material according to claim 1, wherein In the step of pouring the molten copper into the electromagnetic casting crystallizer after it has been allowed to stand, the electromagnetic frequency of the electromagnetic casting crystallizer is 20-25Hz, and the billet is pulled out at a temperature of 360-450℃.
5. The method of preparing a bronze etching material according to claim 1, wherein In the step of performing a first precision rolling and a first tempering on the first billet, the temperature of the first tempering is 650-700°C. In the step of performing a second precision rolling and a second tempering on the second billet, the tempering temperature of the second tempering is 400-500°C.
6. The method of preparing a bronze etching material according to claim 1, wherein In the step of performing a third finishing roll and a third tempering on the third billet, the tempering temperature of the third tempering is 350-450°C. In the steps of performing the fourth finishing rolling and the fourth tempering on the fourth billet, the tempering temperature of the fourth tempering is 230-300℃.
7. The method of preparing a bronze etching material according to claim 1, wherein The step of cleaning and passivating the first finished product includes: The first finished product is cleaned using sulfuric acid, with a concentration of 10.0-15.0%.
Citation Information
Patent Citations
Preparation method of low-plate-type I-value tin-phosphor bronze strip
CN114107727A
Production process of tin-copper alloy strip
CN102069354A