CN104162669A - Technology for preparing metal nickel-silicon nitride ceramic composite material - Google Patents
Technology for preparing metal nickel-silicon nitride ceramic composite material Download PDFInfo
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- CN104162669A CN104162669A CN201410386046.1A CN201410386046A CN104162669A CN 104162669 A CN104162669 A CN 104162669A CN 201410386046 A CN201410386046 A CN 201410386046A CN 104162669 A CN104162669 A CN 104162669A
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Abstract
The invention provides a technology for preparing a metal nickel-silicon nitride ceramic composite material. The technology is characterized by adopting the following steps that (1), a chemical plating technology is used for preparing silicon nitride powder coated with a metal nickel layer, and the thickness of the nickel layer is controlled by controlling the technological parameters such as the sensibilization and activation treatment modes, reducing agents, the composition and the concentration of a plating solution and the chemical plating time in the chemical plating technology; (2), taking ethyl alcohol as a dispersion medium and small silicon nitride balls with the diameter of 2-3 mm as a grinding medium, the silicon nitride powder coated with the metal nickel layer, 3-10 wt.% (calculated according to the amount of the nickel-silicon nitride composite powder) of superfine nickel powder, and 1-3 wt.% (calculated according to the amount of the nickel-silicon nitride composite powder) of activated carbon powder are fast processed in a ball grinding mode in a nylon pot for 30 min and then dried to prepare the mixed powder; (3), the mixed powder is compressed into a block shape through a cold isostatic press at the pressure of 100 MPa; (4), compressed samples are put into a multifunctional sintering furnace for vacuum pressure sintering for 2 h at the pressure of 25 MPa and the temperature of 1600 DEG C, and the vacuum degree is smaller than or equal to 1.0* 10<-2> Pa; (5), the metal nickel-silicon nitride ceramic composite material can be obtained after the furnace is naturally cooled to the room temperature.
Description
Technical field
The preparation technology who the present invention relates to a kind of metallic nickel-silicon nitride ceramics composite, belongs to field of new.
Background technology
Silicon nitride ceramics has many good performances such as intensity is high, hardness is high, high temperature resistant, wear-resistant, corrosion-resistant, density is little, is one of best ceramic material of current toughness, is to have very much the room temperature of development potentiality and the developmental research object of high-temperature structural material.The toughness of silicon nitride ceramics by current various strengthening and toughening mechanism ofs (as, fiber reinforced, crystal whisker toughened, transformation toughening, particulate reinforcement, Nanocomposite are toughness reinforcing) etc. constantly improved, and be used widely on a lot of structural members, but when making flake structure part (as phone housing etc.), the toughening effect that these toughness reinforcing approach reach is still difficult to meet instructions for use, and this flake structure part is higher to the requirement of toughness of material and manufacturing process.As, as the material of mobile phone shell, General Requirements thin slice (thickness≤1mm), intensity is high, wearability good, shock resistance is high, and silicon nitride material advantage makes it have in this respect good application prospect, but still needs to consider to adopt novel toughness reinforcing approach to go to improve its shock resistance.This research adopts the prerequisite of Metal Phase flexible silicon nitride to be based on just preparing this flake structure part that (serviceability temperature is no more than 100 ℃) used under low temperature environment, as phone housing etc.This metal-silicon nitride composite has been avoided the at high temperature oxidizable side effect of metal composite, makes metal improve silicon nitride toughness and the effect that improves sintering character is given full play to.The report of preparing at present metal silicon nitride ceramic composite is considerably less, because prepare nitride metal silicon composite, need to solve a lot of technical barriers, as Metal Phase at silicon nitride in mutually all and distribution problem; The compatible problem of Metal Phase and silicon nitride in high temperature sintering; The problem of Metal Phase stable existence in high temperature sintering, once because Metal Phase is burning till middle generation chemical reaction, remain in crystal boundary with regard to the form that is difficult to continue with Metal Phase, so very easily causes intensity to worsen.Test of many times is passed through in this research, these problems are solved one by one, first utilize chemical plating process to prepare the composite granule of preparing the special use of metallic nickel-silicon nitride ceramics, then utilize vacuum heating-press sintering technique, at suitable temperature, successfully prepared metallic nickel-silicon nitride ceramics composite.
Metallic nickel-ceramic composite powder is the critical materials of preparing metallic nickel toughening ceramic material.Metallic nickel-ceramic composite powder that this research adopts is the beta-silicon nitride powder that adopts the coated nickel of chemical plating processing.Also be one of technological difficulties important in this research and research contents.Prepare at present that metal-ceramic composite powder mainly contains that mechanical mixture, high-energy ball milling, self propagating high temperature are synthetic, reaction in-situ, sol-gel, vapour deposition, chemical plating several method.Adopting chemically plating is the technology of rising the beginning of this century for metallic cover ceramic powder, and chemical plating principle is exactly very simply that the redox reaction of metal simple-substance occurs to generate on powder granule surface, but its process control procedure more complicated.The composite powder of at present existing metallic cover oxide ceramic powder body and carbide ceramics powder, the rare report of silicon nitride powder.Because different powder surface functional groups has bigger difference, in chemical plating fluid, the dynamic process of chemical plating is produced to the different impact of meeting, therefore for each ceramic powder, need to grope different chemical plating process parameters.This research, through test of many times, has been found out a set of chemical plating process that is applicable to efficiently beta-silicon nitride powder covered with metal layer, has successfully prepared at present the coated silicon nitride powder of nickel, and coated metallic nickel content can be controlled within the scope of 1-60wt% as required.The content of clad metal is extremely important to preparing the intensity of metal-silicon nitride ceramic composite.
Sharp bright paper " the Fe coated Si on the journal > > of < < Central South University (from section's version) of silver of Hunan University of Technology
3n
4cermet phase reaction thermodynamic analysis " utilize non-homogeneous phase deposition thermal reduction to prepare Fe coating alpha-Si
3n
4composite powder, and studied its normal pressure-sintered interfacial reaction characteristic.
The Master's thesis of the Liu Zhong of the Chinese Marine University virtue Study on Preparation of beta-silicon nitride powder " nickel coated " adopts chemical plating process, but he utilizes, is that nickel chloride is nickel source, and hydrazine hydrate is reducing agent, and palladium bichloride is activator.And the coated silicon nitride powder of nickel has just been prepared in his research, does not study it and prepares nickel-silicon nitride composite material for sintering.
The existing preparation in nickel-silicon nitride composite powder technology that above-mentioned two pieces of documents are representative, the sharp bright research of silver and the present invention have essential difference, what he adopted is that non-precipitation from homogeneous solution thermal reduction is prepared the coated beta-silicon nitride powder of iron, and the present invention adopts chemical plating process to prepare the coated silicon nitride composite powder of nickel.Though the research of Liu Zhongfang is to adopt chemical plating process, has a lot of significant differences with the present invention.In chemical plating process, the compositional system of chemical plating fluid and the selection of sensitizer are the decisive links of chemical plating success or not, and different chemical plating fluids and sensitizer have conclusive impact to the quality of coating.The chemical plating fluid that Liu Zhongfang adopts is nickel chloride and hydrazine hydrate system, and sensitizer adopts palladium bichloride, and hydrazine hydrate and palladium bichloride are compared with sodium hypophosphite and the more expensive reagent of silver nitrate genus.The nickelous sulfate, the sodium hypophosphite plating solution that in this and the present invention, adopt, and the process detail that silver nitrate is sensitizer has great difference; And in the technique of Liu Zhongfang, chemical plating fluid be nickel source nickel chloride is the mixing mother liquor together with being blended directly in advance with reducing agent hydrazine hydrate, while there is redox reaction in silicon nitride powder surface like this, the generative process of nickel dam is more concentrated, and coated nickel dam there will be phenomenon in uneven thickness; In the present invention, reducing agent sodium hypophosphite adopts the form slowly dripping, and can control so the slow generation of redox reaction, the namely slow generation of nickel dam, and this has very important significance to preparing the nickel dam of even thickness.Moreover in the research of Liu Zhongfang, do not relate to the problem of utilizing the coated silicon nitride powder sintrered nickel silicon nitride composite material of its nickel of preparing.In sintering because solving the problems such as stable existence of nickel, need to carry out great many of experiments from aspects such as determining of formula Design and calcining system, just can resolve the stable existence problem of metallic nickel, this research conducts in-depth research nickel beta-silicon nitride powder sintering, formulates out relatively good formula system and calcining system.
Summary of the invention
The object of the present invention is to provide a kind of technique of preparing metallic nickel-silicon nitride composite material.Its technical scheme is: (1) is first coated with the beta-silicon nitride powder of metal nickel dam with chemical plating process preparation, by controlling sensitization in chemical plating process, activation processing mode, reducing agent, it is thick that the technological parameters such as plating solution composition and concentration and chemical plating time are controlled nickel dam; (2) silicon nitride composite powder of certain metal nickel dam and the extra-fine nickel powder of 3-10wt% will be coated with, 1-3wt.% activated carbon powder, does decentralized medium with ethanol, with diameter, is that 2-3mm silicon nitride bead is done abrasive media, in nylon tank, quick ball milling 30min post-drying, makes mixed powder; (3) by the compressing bulk of cold isostatic press 100MPa for mixed powder; (4), by the sample suppressing, put into multifunctional sintering furnace vacuum pressed sintering, pressure 25MPa; 1600 ℃ of sintering schedules, 2h; Vacuum≤1.0 * 10
-2pa; (5) after furnace temperature is naturally cooling to room temperature, can obtain metallic nickel-silicon nitride composite material.
The described technique of preparing nickel-silicon nitride composite material, the concrete technical process in step (1) is: the former powder of silicon nitride that is 0.3-1 μ m by average grain diameter is put into HNO
3in solution (the ratio 1:3 of red fuming nitric acid (RFNA) and distilled water), stir 6-10h, this process is alligatoring; Beta-silicon nitride powder after alligatoring is separated, and puts into the SnCl that concentration is 15-30g/l
2and HNO
3mixed solution (red fuming nitric acid (RFNA) consumption is 30-45ml/l) in, 50 ℃ are stirred 6h, this process is sensitization; Silicon nitride powder after sensitization is complete is separated, and puts into the AgNO that concentration is 0.5-2g/l
3and HNO
3mixed solution (red fuming nitric acid (RFNA) consumption is 150-250ml/l) in stirring at room 6h, this process cry to activate; Silicon nitride powder after activation is separated, the NiSO that to put into by concentration be 50-80g/l
4in, with NaOH, regulating pH is 11, and the acetic acid that cushioning liquid is 20-30g/l by concentration-sodium acetate forms, and then stirring at normal temperature 0.5h drips the NaH that a certain amount of (used in amounts is calculated according to the former powder amount of added silicon nitride) concentration is 30-60g/l in system
2pO
2, stir on dropping limit, limit, time for adding 1h left and right, in process, system temperature is controlled at 70 ℃ of left and right, drips at latter 70 ℃ and continues to stir 6-10h, and this process is chemical plating, silicon nitride powder after having plated is separated, and can obtain being coated with the beta-silicon nitride powder of metal nickel dam.
The described technique of preparing metallic nickel-silicon nitride composite material, needs to add extra-fine nickel powder and the 1-3wt.% activated carbon powder of 3-10wt% in step (2).
The described technique of preparing metallic nickel-silicon nitride composite material, the sintering temperature in step (4) is generally determined according to the kind of silicon nitride powder surface institute clad metal; The sintering schedule of determining nickel-silicon nitride ceramic material is a complicated process, need to carry out repeatedly sintered specimen and determine.If the fusing point of nickel is 1453 ℃, if but at this temperature sintering, nickel is easy to and silicon nitride generates NiSi, NiSi
2, now, NiSi, NiSi
2not yet carrying out a large amount of reactions with C, is mainly NiSi, NiSi in crystal boundary
2phase, it is less that metallic nickel keeps, and causes the intensity of sample not high; And when temperature rises to more than 1600 ℃, NiSi, NiSi
2start to generate in a large number Ni and SiC with the C adding, now, because keeping higher vacuum in stove, the maintenance that nickel just can be stable exists, and the intensity of sample is improved greatly.
Technological principle of the present invention: ceramic-metallic Toughening Mechanism has been used for reference in this research, propose to adopt the metallic nickel with good ductility to carry out mutually malleableize silicon nitride ceramics as combination, first by the coated layer of metal nickel dam in silicon nitride powder surface, the metallic nickel particle of certain mass percent is mixed in the nitrogenize powder material that is coated with nickel dam simultaneously, by selecting suitable vacuum hotpressing calcining system, the maintenance that metallic nickel can be stable between silicon nitride particle after burning till is existed, formation has the metal crystal boundary of certain ductility, the mechanism of utilizing the plastic deformation of metal to absorb energy to failure improves the toughness of material.Prepare like this nickel-silicon nitride composite material with excellent impact resistance energy and high-strength wearable using under low temperature environment.
The specific embodiment
embodiment 1:
Step 1: prepare the coated silicon nitride powder of nickel with chemical plating process.First use certain density HNO
3solution (red fuming nitric acid (RFNA): distilled water is 1:3) is the former powder alligatoring of 0.5 μ m silicon nitride 10h by average grain diameter; By the former powder after alligatoring, the SnCl that is 15g/l in concentration
2with rare HNO
3mixed solution (red fuming nitric acid (RFNA) consumption is 40ml/l) in sensitization 6h; Then the silicon nitride powder after sensitization being put into concentration is 0.6g/lAgNO
3and HNO
3mixed solution (red fuming nitric acid (RFNA) consumption is 150ml/l) in activation 6h; Finally the silicon nitride powder after activation being put into by concentration is 50g/l NiSO
4in, regulating pH is 11, slowly drips the NaH that concentration is 35g/l
2pO
2solution, and stir 6 hours under 70 ℃ of heating water baths, finally powder is leached to oven dry, can obtain the beta-silicon nitride powder of coated certain thickness nickel dam.
Step 2: take a certain amount of above-mentioned silicon nitride fine powder that is coated with nickel dam, then calculate according to the silicon nitride powder gross mass of coated nickel used, take nickel powder and the 1wt% activated carbon powder of 3wt%.
Step 3: the silicon nitride powder of the coated nickel weighing up, metal nickel powder and activated carbon powder are put into nylon ball grinder, do decentralized medium with ethanol, 2-3mm silicon nitride ball, as ball-milling medium, after ball milling 30min, is dried and obtains mixed powder fast.
Step 4: by mixed powder cold isostatic press, briquet under 100MPa; (3), by the block sample suppressing, put into multifunctional sintering furnace vacuum pressed sintering, pressure 25MPa; 1600 ℃ of sintering schedules, 2h, vacuum≤1.0 * 10
-2pa.
Step 5: to room temperature, can obtain nickel-silicon nitride composite material after furnace temperature is naturally cooling.
embodiment 2:
Step 1: prepare the coated silicon nitride powder of nickel with chemical plating process.First use certain density HNO
3solution (red fuming nitric acid (RFNA): distilled water is 1:3) is the former powder alligatoring of 0.5 μ m silicon nitride 10h by average grain diameter; By the former powder after alligatoring, the SnCl that is 20g/l in concentration
2with rare HNO
3mixed solution (red fuming nitric acid (RFNA) consumption is 40ml/l) in sensitization 6h; Then the silicon nitride powder after sensitization being put into concentration is 1.0g/lAgNO
3and HNO
3mixed solution (red fuming nitric acid (RFNA) consumption is 150ml/l) in activation 6h; Finally the silicon nitride powder after activation being put into by concentration is 60g/l NiSO
4in, regulating pH is 11, slowly drips the NaH that concentration is 45g/l
2pO
2solution, and stir 8 hours under 70 ℃ of heating water baths, finally powder is leached to oven dry, can obtain the beta-silicon nitride powder of coated certain thickness nickel dam.
Step 2: take a certain amount of above-mentioned silicon nitride fine powder that is coated with nickel dam, then calculate according to the silicon nitride powder gross mass of coated nickel used, take nickel powder and the 2wt% activated carbon powder of 5wt%.
Step 3: the silicon nitride powder of the coated nickel weighing up, metal nickel powder and activated carbon powder are put into nylon ball grinder, do decentralized medium with ethanol, 2-3mm silicon nitride ball, as ball-milling medium, after ball milling 30min, is dried and obtains mixed powder fast.
Step 4: by mixed powder cold isostatic press, briquet under 100MPa; (3), by the block sample suppressing, put into multifunctional sintering furnace vacuum pressed sintering, pressure 25MPa; 1600 ℃ of sintering schedules, 2h, vacuum≤1.0 * 10
-2pa.
Step 5: to room temperature, can obtain nickel-silicon nitride composite material after furnace temperature is naturally cooling.
embodiment 3:
Step 1: prepare the coated silicon nitride powder of nickel with chemical plating process.First use certain density HNO
3solution (red fuming nitric acid (RFNA): distilled water is 1:3) is the former powder alligatoring of 0.5 μ m silicon nitride 10h by average grain diameter; By the former powder after alligatoring, the SnCl that is 25g/l in concentration
2with rare HNO
3mixed solution (red fuming nitric acid (RFNA) consumption is 40ml/l) in sensitization 6h; Then the silicon nitride powder after sensitization being put into concentration is 1.5g/lAgNO
3and HNO
3mixed solution (red fuming nitric acid (RFNA) consumption is 150ml/l) in activation 6h; Finally the silicon nitride powder after activation being put into by concentration is 70g/l NiSO
4in, regulating pH is 11, slowly drips the NaH that concentration is 50g/l
2pO
2solution, and stir 10 hours under 70 ℃ of heating water baths, finally powder is leached to oven dry, can obtain the beta-silicon nitride powder of coated certain thickness nickel dam.
Step 2: take a certain amount of above-mentioned silicon nitride fine powder that is coated with nickel dam, then calculate according to the silicon nitride powder gross mass of coated nickel used, take nickel powder and the 3wt% activated carbon powder of 7wt%.
Step 3: the silicon nitride powder of the coated nickel weighing up, metal nickel powder and activated carbon powder are put into nylon ball grinder, do decentralized medium with ethanol, 2-3mm silicon nitride ball, as ball-milling medium, after ball milling 30min, is dried and obtains mixed powder fast.
Step 4: by mixed powder cold isostatic press, briquet under 100MPa; (3), by the block sample suppressing, put into multifunctional sintering furnace vacuum pressed sintering, pressure 25MPa; 1600 ℃ of sintering schedules, 2h, vacuum≤1.0 * 10
-2pa.
Step 5: to room temperature, can obtain nickel-silicon nitride composite material after furnace temperature is naturally cooling.
embodiment 4:
Step 1: prepare the coated silicon nitride powder of nickel with chemical plating process.First use certain density HNO
3solution (red fuming nitric acid (RFNA): distilled water is 1:3) is the former powder alligatoring of 0.5 μ m silicon nitride 10h by average grain diameter; By the former powder after alligatoring, the SnCl that is 30g/l in concentration
2with rare HNO
3mixed solution (red fuming nitric acid (RFNA) consumption is 40ml/l) in sensitization 6h; Then the silicon nitride powder after sensitization being put into concentration is 2g/lAgNO
3and HNO
3mixed solution (red fuming nitric acid (RFNA) consumption is 150ml/l) in activation 6h; Finally the silicon nitride powder after activation being put into by concentration is 80g/l NiSO
4in, regulating pH is 11, slowly drips the NaH that concentration is 60g/l
2pO
2solution, and stir 10 hours under 70 ℃ of heating water baths, finally powder is leached to oven dry, can obtain the beta-silicon nitride powder of coated certain thickness nickel dam.
Step 2: take a certain amount of above-mentioned silicon nitride fine powder that is coated with nickel dam, then calculate according to the silicon nitride powder gross mass of coated nickel used, take nickel powder and the 3wt% activated carbon powder of 10wt%.
Step 3: the silicon nitride powder of the coated nickel weighing up, metal nickel powder and activated carbon powder are put into nylon ball grinder, do decentralized medium with ethanol, 2-3mm silicon nitride ball, as ball-milling medium, after ball milling 30min, is dried and obtains mixed powder fast.
Step 4: by mixed powder cold isostatic press, briquet under 100MPa; (3), by the block sample suppressing, put into multifunctional sintering furnace vacuum pressed sintering, pressure 25MPa; 1600 ℃ of sintering schedules, 2h, vacuum≤1.0 * 10
-2pa.
Step 5: to room temperature, can obtain nickel-silicon nitride composite material after furnace temperature is naturally cooling.
Claims (4)
1. a preparation technology for nickel-silicon nitride composite material, is characterized in that adopting following steps: (1) is first coated with the beta-silicon nitride powder of metal nickel dam with chemical plating process preparation; Concrete technical process is: the former powder of silicon nitride that is 0.3-1 μ m by average grain diameter is put into HNO
3in solution (the ratio 1:3 of red fuming nitric acid (RFNA) and distilled water), stir 6-10h, this process is alligatoring; Beta-silicon nitride powder after alligatoring is separated, and puts into the SnCl that concentration is 15-30g/l
2and HNO
3mixed solution (red fuming nitric acid (RFNA) consumption is 30-45ml/l) in, 50 ℃ are stirred 6h, this process is sensitization; Silicon nitride powder after sensitization is complete is separated, and puts into the AgNO that concentration is 0.5-2g/l
3and HNO
3mixed solution (red fuming nitric acid (RFNA) consumption is 150-250ml/l) in stirring at room 6h, this process cry to activate; Silicon nitride powder after activation is separated, the NiSO that to put into by concentration be 50-80g/l
4in, with NaOH, regulating pH is 11, and the acetic acid that cushioning liquid is 20-30g/l by concentration-sodium acetate forms, and then stirring at normal temperature 0.5h drips the NaH that a certain amount of (used in amounts is calculated according to the former powder amount of added silicon nitride) concentration is 30-60g/l in system
2pO
2, stir on dropping limit, limit, time for adding 1h left and right, in process, system temperature is controlled at 70 ℃ of left and right, drips at latter 70 ℃ and continues to stir 6-10h, and this process is chemical plating, silicon nitride powder after having plated is separated, and can obtain being coated with the beta-silicon nitride powder of metal nickel dam; (2) silicon nitride composite powder of certain metal nickel dam and the extra-fine nickel powder of 3-10wt.% will be coated with, 1-3wt.% activated carbon powder, does decentralized medium with ethanol, with diameter, is that 2-3mm silicon nitride bead is done abrasive media, in nylon tank, quick ball milling 30min post-drying, makes mixed powder; (3) by the compressing bulk of cold isostatic press 100MPa for mixed powder; (4), by the sample suppressing, put into multifunctional sintering furnace vacuum pressed sintering, pressure 25MPa; 1600 ℃ of sintering schedules, 2h; Vacuum≤1.0 * 10
-2pa; (5) after furnace temperature is naturally cooling to room temperature, can obtain metallic nickel-silicon nitride composite material.
2. the technique of nickel-silicon nitride composite material according to claim 1, is characterized in that: in the chemical plating process in (1), activator adopts silver nitrate, and optimum concentration range is 0.5-2g/l; Bath system is nickelous sulfate-ortho phosphorous acid sodium solution, and the form that inferior sodium phosphate adopt to drip adds, and is not directly and nickelous sulfate mixing; Nickelous sulfate optimum concentration range is 50-80g/l; NaH
2pO
2optimum concentration range 30-60g/l; Optimum chemical plating temperature is 70 ℃; Optimum chemical plating reaction time 6-10h.
3. the technique of nickel-silicon nitride composite material according to claim 1, is characterized in that: in (2), need to add the extra-fine nickel powder of 3-10wt%, 1-3wt.% activated carbon powder.
4. the technique of nickel-silicon nitride composite material according to claim 1, is characterized in that: in (4), need to adopt vacuum heating-press sintering, and best sintering schedule is: pressure 25MPa; 1600 ℃ of sintering schedules, 2h; Vacuum≤1.0 * 10
-2pa.
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| CN112553590A (en) * | 2020-12-02 | 2021-03-26 | 上海征世科技有限公司 | Diamond film based on plasma vapor deposition and preparation method thereof |
| CN112553590B (en) * | 2020-12-02 | 2021-07-06 | 上海征世科技股份有限公司 | Diamond film based on plasma vapor deposition and preparation method thereof |
| CN113149677A (en) * | 2021-04-29 | 2021-07-23 | 陕西科技大学 | Nickel wire toughened silicon nitride-based ceramic with wood-like ring structure and preparation method and application thereof |
| CN113213947A (en) * | 2021-05-28 | 2021-08-06 | 福建臻璟新材料科技有限公司 | Aluminum nitride doped modified nano silicon nitride composite ceramic powder and preparation method thereof |
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