CN114686801A - Novel powder zinc impregnation and infiltration assisting process - Google Patents

Novel powder zinc impregnation and infiltration assisting process Download PDF

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Publication number
CN114686801A
CN114686801A CN202210409593.1A CN202210409593A CN114686801A CN 114686801 A CN114686801 A CN 114686801A CN 202210409593 A CN202210409593 A CN 202210409593A CN 114686801 A CN114686801 A CN 114686801A
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Prior art keywords
zincizing
steel member
temperature
zinc impregnation
zinc
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CN202210409593.1A
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CN114686801B (en
Inventor
陈镇平
罗贯虹
马传河
李瑞平
罗长虹
陈秀香
谢华标
李伟良
余煜玺
张飒
杨婉嫆
周俞彤
丘丽华
胡瑞才
邓丽琴
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Fujian Hongguan Roads & Bridge Anti Corrosive Technology Co ltd
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Fujian Hongguan Roads & Bridge Anti Corrosive Technology Co ltd
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    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C10/00Solid state diffusion of only metal elements or silicon into metallic material surfaces
    • C23C10/28Solid state diffusion of only metal elements or silicon into metallic material surfaces using solids, e.g. powders, pastes
    • C23C10/34Embedding in a powder mixture, i.e. pack cementation
    • C23C10/36Embedding in a powder mixture, i.e. pack cementation only one element being diffused
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C10/00Solid state diffusion of only metal elements or silicon into metallic material surfaces
    • C23C10/02Pretreatment of the material to be coated
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C10/00Solid state diffusion of only metal elements or silicon into metallic material surfaces
    • C23C10/60After-treatment
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Preventing Corrosion Or Incrustation Of Metals (AREA)

Abstract

A novel powder zinc impregnation and infiltration assisting process relates to the technical field of metal rust prevention and comprises the following steps: 1) zinc impregnation pretreatment: carrying out surface oil and rust removal treatment on the steel member; 2) embedding a steel member: burying a steel member in a zincizing agent and placing the steel member in a zincizing furnace; 3) and (3) zinc impregnation: heating and rotating the zincizing furnace, and introducing ultrasonic waves and circulating atmosphere in the zincizing process; 4) zinc impregnation post-treatment: and cleaning the galvanized steel member to obtain the multi-element powder co-galvanized steel member. On the basis of the mechanical energy assisted powder zincing method, the invention introduces the second mechanical energy, accelerates the zincing reaction, reduces the zincing time and realizes high-efficiency zincing.

Description

Novel powder zinc impregnation and infiltration assisting process
Technical Field
The invention relates to the technical field of metal rust prevention, in particular to a novel powder zinc impregnation assisting process.
Background
Nowadays, metals have a wide range of applications in people's lives. Accordingly, corrosion prevention of metals is also becoming a considerable problem. The corrosion of metal not only consumes indispensable natural resources in human life, but also seriously damages the normal operation of many activities such as natural environment, industrial production, human life and the like, and the huge economic loss and the serious environmental pollution caused by the corrosion become one of the important factors influencing the modern society and the economic sustainable development. In order to deal with the corrosion of metal, especially to delay the corrosion of metal in a severe working environment, a plurality of methods are adopted to deal with the problem, and the traditional methods comprise oil coating, electroplating, single coating and the like. At present, the method of coating the surface with the anti-rust oil is difficult to maintain the anti-rust performance of the metal component for a long time under severe outdoor conditions, and the traditional processes of electroplating, single zinc-chromium coating and the like are difficult to meet the use requirements of metal parts. This has prompted the search for new corrosion protection technologies.
The powder zincizing technology is to form a zinc-iron alloy layer on the surface of a substrate by utilizing mutual diffusion of zinc and iron atoms, plays a good role in protection and is widely applied to the field of corrosion prevention of steel parts. The powder zincizing chemical heat treatment process obtains zinc-iron alloy on the surface of steel by a thermal diffusion method, and compared with the traditional galvanizing process, the powder zincizing chemical heat treatment process has the advantages of good coating thickness uniformity, high hardness, wear resistance and the like, and the coating thickness is not influenced by the shape and position of a member. However, the problems of slow diffusion speed, long reaction time, high energy consumption, low efficiency and the like exist in the powder zincizing heat treatment process, and the existing zincizing process needs to be optimized and improved or other processes are tried to be developed so as to realize the zincizing with low cost, high quality and high efficiency.
Disclosure of Invention
The invention aims to solve the problems of low diffusion speed, long reaction time, high energy consumption and low efficiency in the zinc process in the prior art, and provides a novel powder zinc impregnation assisting process, which adopts a method of assisting the impregnation by using two mechanical energy of controllable atmosphere and rotation to improve the zinc impregnation efficiency, and simultaneously uses ultrasonic waves and vibration pressure to promote the impregnation during the zinc impregnation, thereby shortening the zinc impregnation time and improving the efficiency and quality of the zinc impregnation process.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention relates to a novel powder zinc impregnation assisting process, which comprises the following steps:
(1) zinc impregnation pretreatment: carrying out surface oil and rust removal treatment on the steel member;
(2) embedding a steel member: burying a steel member in a zincizing agent and placing the zincizing agent in a zincizing furnace;
(3) and (3) zinc impregnation: heating and rotating the zincizing furnace, and introducing ultrasonic waves and circulating atmosphere in the zincizing process;
(4) zinc impregnation post-treatment: and cleaning the galvanized steel member to obtain the multi-element powder co-galvanized steel member.
The oil removal is carried out by preserving the heat of the steel member for 30-60 min at 300-400 ℃ by adopting a high-temperature carbonization oil removal method until the surface of the steel member is free of oil.
The rust removal is shot blasting rust removal, and the rust removal is carried out for 20-30 min under the condition of 0.2-0.4 MPa of compressed air.
The zinc penetrating agent is prepared by adding 70-74% of zinc powder, 3-5% of a penetration assisting agent and 21-27% of quartz sand according to the proportion of a formula.
The temperature is increased from normal temperature to 250-300 ℃ slowly, the temperature is maintained for 20-30 min, then the temperature is increased rapidly to 410-420 ℃ and maintained for 3-5 h, then the temperature is decreased slowly to 250-300 ℃ and maintained for 20-30 min, and finally when the temperature is cooled to 100 ℃, the zincizing furnace is opened and cooled to room temperature along with the furnace.
The rotation is that the rotation number is set to be 5-10 r/min before temperature rise, the rotation number is set to be 10-15 r/min when the temperature rises to 250-300 ℃, the rotation number is set to be 15-20 r/min after the temperature rises to 410-420 ℃, the rotation number is set to be 10-15 r/min when the temperature drops to 250-300 ℃, and the rotation speed is set to be 5-10 r/min when the temperature drops to 100 ℃.
In the invention, the rotating machinery can dynamically assist the control of the revolution of the motor in the seepage, high and low revolution cycles are adopted, and the revolution is changed along with the change of temperature.
The ultrasonic process is characterized in that an ultrasonic motor control under the control of self-adaptive fuzzy logic PID is additionally arranged in the furnace, the parameters are that low-frequency sound waves of 5-10 kHz are applied at the initial stage, the frequency is adjusted to 25-30 kHz at the middle stage, and the frequency is adjusted back to 5-10 kHz at the later stage.
The circulating atmosphere is a controllable atmosphere taking nitrogen as a gas source, the nitrogen flow is 5500-6000L/h, the supply pressure is 0.35-0.45 Mpa, and the nitrogen is used as an inert gas and is used as a blowing gas and a protective gas of the system.
Compared with the prior art, the technical scheme of the invention has the following beneficial effects:
1. on the basis of the mechanical energy assisted powder zincing method, the invention introduces the second mechanical energy, accelerates the zincing reaction, reduces the zincing time and realizes high-efficiency zincing.
2. The invention adopts ultrasonic wave to spread penetrating agent in the zincizing furnace to act on the component to achieve the effect of enhancing diffusion, the power of the component changes from small to large and from small along with the change of zincizing temperature, and the property and the state of the zincizing component can be changed to increase the diffusion coefficient of the component.
3. According to the invention, the volume content of oxygen in the furnace can be controlled through the circulating atmosphere, and the zinc powder is prevented from being rapidly oxidized under the condition of temperature rise, wherein the circulating atmosphere mode is closed circulating type air blowing, an air blower, a ventilation pipe and a receiving device are additionally arranged in the zinc impregnation furnace, so that air flow is circulated in the furnace, and the air blowing mode is closed circulating type, so that heat dissipation and impregnation agent loss can be avoided.
4. The parameter circulation setting adopted by the invention is beneficial to the absorption of zinc powder and the improvement of the zinc impregnation efficiency; the process reduces the energy consumption and the use of resources, and simultaneously improves the uniformity, the corrosivity and the wear resistance of the zincizing layer.
Detailed Description
To further illustrate the technical means and effects of the present invention adopted to achieve the predetermined objects, the following detailed description will be given to the specific implementation, structure, features and effects of the novel powder zincing infiltration assisting process provided by the present invention in combination with the preferred embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention. Furthermore, the particular features, structures, or characteristics may be combined in any suitable manner in one or more embodiments.
Example 1:
(1) zinc impregnation pretreatment: the workpiece is kept at 300 ℃ for 30min by adopting a high-temperature carbonization oil removal method, and is treated for 20min under the atmospheric pressure of 0.2MPa by utilizing a shot blasting rust removal process.
(2) Embedding a steel member: the steel member is placed in a zinc impregnation furnace, and 70% of zinc powder, 4% of a permeation aid and 26% of quartz sand are added according to the proportion of the formula to embed the steel member.
(3) And (3) zinc impregnation: rotating the zincizing furnace, adding circulating controllable nitrogen, with the air flow being 5500L/h and the pressure being 0.35 Mpa. Adding an ultrasonic motor controlled by self-adaptive fuzzy logic PID in the furnace, starting a temperature control program and an ultrasonic program of the zincizing furnace, setting the revolution of the zincizing furnace to be 5r/min before heating, the ultrasonic frequency to be 5kHz, the initial heating rate to be 3 ℃/min, adjusting the rotating speed to be 10r/min after heating to 250 ℃, adjusting the rotating speed to be 15r/min after adjusting the heating rate to be 5 ℃/min to be 410 ℃, adjusting the ultrasonic frequency to be 25kHz, preserving heat for 5h, adjusting the rotating speed to be 10r/min after adjusting the cooling rate to be 5 ℃/min to be 250 ℃, adjusting the ultrasonic frequency to be 5kHz, preserving heat for 30min, adjusting the rotating speed to be 5r/min after adjusting the cooling rate to be 3 ℃/min to 100 ℃, closing a temperature control system, and idling the infiltration piece along with the furnace to cool to obtain the infiltration piece.
(4) Zinc impregnation post-treatment: and cleaning the galvanized steel member to obtain the multi-element powder co-galvanized steel member.
Example 2:
(1) zinc impregnation pretreatment: the workpiece is kept warm for 40min at 350 ℃ by adopting a high-temperature carbonization degreasing method, and is treated for 30min under the atmospheric pressure of 0.3MPa by utilizing a shot blasting rust removal process.
(2) Embedding a steel member: the steel member is placed in a zinc impregnation furnace, and 72% of zinc powder, 3% of a permeation aid and 25% of quartz sand are added according to the formula proportion to embed the steel member.
(3) And (3) zinc impregnation: rotating the zincizing furnace, adding circulating controllable nitrogen, with the air flow being 5500L/h and the pressure being 0.35 Mpa. Adding an ultrasonic motor controlled by self-adaptive fuzzy logic PID in the furnace, starting a temperature control program and an ultrasonic program of the zincizing furnace, setting the revolution of the zincizing furnace to be 10r/min before heating, the ultrasonic frequency to be 5kHz, the initial heating rate to be 3 ℃/min, adjusting the rotating speed to be 15r/min after heating to 250 ℃, adjusting the rotating speed to be 20r/min after adjusting the heating rate to be 5 ℃/min to be 410 ℃, adjusting the ultrasonic frequency to be 25kHz, preserving heat for 5h, adjusting the rotating speed to be 15r/min after adjusting the cooling rate to be 5 ℃/min to be 250 ℃, adjusting the ultrasonic frequency to be 5kHz, preserving heat for 30min, adjusting the rotating speed to be 10r/min after adjusting the cooling rate to be 3 ℃/min to 100 ℃, closing a temperature control system, and idling the infiltration piece along with the furnace to cool to obtain the infiltration piece.
(4) Zinc impregnation post-treatment: and cleaning the galvanized steel member to obtain the multi-element powder co-galvanized steel member.
Example 3:
(1) zinc impregnation pretreatment: the workpiece is kept at 400 ℃ for 60min by adopting a high-temperature carbonization oil removal method, and is treated for 30min under the atmospheric pressure of 0.4MPa by utilizing a shot blasting rust removal process.
(2) Embedding a steel member: the steel member is placed in a zinc impregnation furnace, and 74% of zinc powder, 4% of a permeation aid and 22% of quartz sand are added according to the proportion of the formula to embed the steel member.
(3) And (3) zinc impregnation: rotating the zincizing furnace, adding circulating controllable nitrogen, with the air flow being 5500L/h and the pressure being 0.35 Mpa. Adding an ultrasonic motor controlled by self-adaptive fuzzy logic PID in the furnace, starting a temperature control program and an ultrasonic program of the zincizing furnace, setting the revolution of the zincizing furnace to be 10r/min before heating, the ultrasonic frequency to be 10kHz, the initial heating rate to be 3 ℃/min, adjusting the rotating speed to be 15r/min after heating to 300 ℃, adjusting the rotating speed to be 20r/min after adjusting the heating rate to be 5 ℃/min to be 420 ℃, adjusting the ultrasonic frequency to be 30kHz, preserving heat for 3h, adjusting the rotating speed to be 15r/min after adjusting the cooling rate to be 5 ℃/min to be 300 ℃, adjusting the ultrasonic frequency to be 10kHz, preserving heat for 30min, adjusting the rotating speed to be 10r/min after adjusting the cooling rate to be 3 ℃/min to 100 ℃, closing a temperature control system, and idling the infiltration piece along with the furnace to cool to obtain the infiltration piece.
(4) Zinc impregnation post-treatment: and cleaning the galvanized steel member to obtain the multi-element powder co-galvanized steel member.
The thickness of the penetrating layer of the penetrating member prepared in the embodiment 1-3 is 80-140 μm, and the heat preservation time is far shorter than the zinc penetrating time for preparing the zinc penetrating layer with the same thickness.
In summary, the invention introduces ultrasonic waves and inert atmosphere, and simultaneously uses mechanical energy application modes with different rotating speeds, thereby improving the powder zincification efficiency and the zincification thickness.

Claims (8)

1. A novel powder zinc impregnation and infiltration assisting process is characterized by comprising the following steps:
1) zinc impregnation pretreatment: carrying out surface oil and rust removal treatment on the steel member;
2) embedding a steel member: burying a steel member in a zincizing agent and placing the steel member in a zincizing furnace;
3) and (3) zinc impregnation: heating and rotating the zincizing furnace, and introducing ultrasonic waves and circulating atmosphere in the zincizing process;
4) zinc impregnation post-treatment: and cleaning the galvanized steel member.
2. The novel powder zincizing and infiltration assisting process of claim 1, which is characterized in that: in the step 1), the oil removal is carried out by a high-temperature carbonization oil removal method, and the steel member is kept at 300-400 ℃ for 30-60 min until the surface of the steel member has no oil.
3. The novel powder zincizing and infiltration assisting process of claim 1, which is characterized in that: in the step 1), the rust removal is shot blasting rust removal, and the rust removal is carried out for 20-30 min under the condition of 0.2-0.4 MPa of compressed air.
4. The novel powder zincizing and infiltration assisting process of claim 1, which is characterized in that: in the step 2), 70-74% of zinc powder, 3-5% of permeation-assistant agent and 21-27% of quartz sand are added into the zinc-infiltrating agent according to the proportion of the formula.
5. The novel powder zincizing and infiltration assisting process of claim 1, which is characterized in that: in the step 3), the temperature is slowly increased from the normal temperature to 250-300 ℃, the temperature is maintained for 20-30 min, then the temperature is quickly increased to 410-420 ℃, the temperature is maintained for 3-5 h, then the temperature is slowly decreased to 250-300 ℃, the temperature is maintained for 20-30 min, and finally the cooling is carried out.
6. The novel powder zincizing and cementation assisting process as claimed in claim 1 or 5, wherein: in the step 3), the rotation is that the rotation number is set to be 5-10 r/min before temperature rise, the rotation number is set to be 10-15 r/min when the temperature rises to 250-300 ℃, the rotation number is set to be 15-20 r/min after the temperature rises to 410-420 ℃, the rotation number is set to be 10-15 r/min when the temperature drops to 250-300 ℃, and the rotation number is set to be 5-10 r/min during cooling.
7. The novel powder zincizing and infiltration assisting process of claim 1, which is characterized in that: in the step 3), the introduced ultrasonic wave is controlled by an ultrasonic motor additionally arranged in the furnace and controlled by an adaptive fuzzy logic PID, the parameters are that low-frequency sound waves of 5-10 kHz are applied in the initial stage, the frequency is adjusted to 25-30 kHz in the middle stage, and the frequency is adjusted back to 5-10 kHz in the later stage, so that the ultrasonic wave is transmitted in the zincizing furnace to penetrate through the penetrating agent to act on the member to enhance diffusion.
8. The novel powder zincizing and infiltration assisting process of claim 1, which is characterized in that: in the step 3), the circulating atmosphere adopts a controllable atmosphere taking nitrogen as a gas source, the flow of the nitrogen is 5500-6000L/h, and the pressure supply pressure is 0.35-0.45 Mpa.
CN202210409593.1A 2022-04-19 2022-04-19 Powder zinc impregnation and permeation assisting process Active CN114686801B (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20100086680A1 (en) * 2008-10-02 2010-04-08 Rolls-Royce Corp. Mixture and technique for coating an internal surface of an article
CN103526155A (en) * 2013-10-11 2014-01-22 昆明理工大学 Preparation method for oxide dispersion iron aluminum alloy coating
CN107142446A (en) * 2017-04-28 2017-09-08 南宁普来得工贸有限公司 Powder zinc impregnation finished piece with high hardness and strong corrosion resistance
CN110343997A (en) * 2019-08-07 2019-10-18 郑州中原利达新材料有限公司 A kind of powder zincizing penetration-assisting agent
CN112853260A (en) * 2021-01-09 2021-05-28 华东理工大学 Preparation method of powder embedding infiltration coating

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20100086680A1 (en) * 2008-10-02 2010-04-08 Rolls-Royce Corp. Mixture and technique for coating an internal surface of an article
CN103526155A (en) * 2013-10-11 2014-01-22 昆明理工大学 Preparation method for oxide dispersion iron aluminum alloy coating
CN107142446A (en) * 2017-04-28 2017-09-08 南宁普来得工贸有限公司 Powder zinc impregnation finished piece with high hardness and strong corrosion resistance
CN110343997A (en) * 2019-08-07 2019-10-18 郑州中原利达新材料有限公司 A kind of powder zincizing penetration-assisting agent
CN112853260A (en) * 2021-01-09 2021-05-28 华东理工大学 Preparation method of powder embedding infiltration coating

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Title
黄建洪;: "影响化学热处理中原子扩散的因素―物理因素(Ⅰ)", 热处理, no. 05 *

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