CN104162669B - A kind of technique for preparing metallic nickel-silicon nitride ceramics composite material - Google Patents
A kind of technique for preparing metallic nickel-silicon nitride ceramics composite material Download PDFInfo
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Abstract
The present invention provides a kind of preparation process of nickel silicon nitride composite material.It is characterized in that using following steps：（1）First prepared with chemical plating process and be coated with the beta-silicon nitride powder of metal nickel layer, by controlling sensitization, activation process mode in chemical plating process, reducing agent, the technological parameter such as plating solution composition and concentration and electroless plating time controls nickel layer thick；（2）The silicon nitride composite powder and 3 10wt.% of certain metal nickel layer will be coated with（Calculated according to nickel silicon nitride composite powder dosage）Extra-fine nickel powder, 1 3wt.%（Calculated according to nickel silicon nitride composite powder dosage）Active powdered carbon, decentralized medium is done with ethanol, and abrasive media is done with a diameter of 2 3mm silicon nitride beads, is dried in nylon tank after quick ball milling 30min, mixed powder is made；（3）By the mixed powder compressing bulks of cold isostatic press 100MPa；（4）The sample that will be suppressed, is put into vacuum pressed in multifunctional sintering furnace and sinters, pressure 25MPa；1600 DEG C of sintering schedule, 2h；Vacuum≤1.0 × 10‑2Pa；（5）To after room temperature after furnace temperature natural cooling, you can obtain metallic nickel silicon nitride composite material.
Description
Technical field
The present invention relates to a kind of preparation process of metallic nickel-silicon nitride ceramics composite material, belong to field of new materials.
Background technology
Many excellent property such as silicon nitride ceramics has intensity height, hardness height, high temperature resistant, wear-resistant, corrosion-resistant, density is small
Can, it is one of best ceramic material of current toughness, is the developmental research for the room temperature and high-temperature structural material for having very much development potentiality
Object.The toughness of silicon nitride ceramics by current various strengthening and toughening mechanism ofs (e.g., fiber reinforced, crystal whisker toughened, transformation toughening,
Particulate reinforcement, Nanocomposite toughness reinforcing) etc. constantly improving, and be used widely on many structural members, but making
During flake structure part (such as phone housing), the toughening effect that these toughness reinforcing approach are reached still is difficult to meet requirement,
Requirement higher of this flake structure part to toughness of material and manufacturing process.Such as, the material as mobile phone shell, generally requires thin slice
(thickness≤1mm), intensity is high, wearability is good, and shock resistance is high, and silicon nitride material advantage causes it to have in this respect well
Application prospect, but still need to be considered as new toughness reinforcing approach to go to improve its shock resistance.This research is increased using metal phase
The premise of tough silicon nitride is exactly based on the thin slice knot for preparing this (temperature in use no more than 100 DEG C) at low ambient temperatures and using
Component, such as phone housing.This metal-Nitride silicon composite avoids the secondary work oxidizable at high temperature of metal composite
With, enable metal improve silicon nitride toughness and improve sintering character effect give full play to.Metal silicon nitride pottery is prepared at present
The report of porcelain composite material is considerably less, because preparing nitride metal silicon composite needs to solve many technical barriers, such as metal
The mutually equal and distribution problem in silicon nitride phase；Metal phase and the compatible problem of silicon nitride in high temperature sintering；It is golden in high temperature sintering
The problem of symbolic animal of the birth year is stabilized, once because metal phase chemically reacts in burning till, is just difficult to continue with the shape of metal phase
Formula is maintained in crystal boundary, so easily causes strength deterioration.This research passes through test of many times, these problems are understood one by one
Certainly, prepared first with chemical plating process and prepared the dedicated composite granule of metallic nickel-silicon nitride ceramics, then utilized vacuum
Hot-pressing sintering technique, is successfully prepared metallic nickel-silicon nitride ceramics composite material at a suitable temperature.
Metallic nickel-ceramic composite powder is the critical materials for preparing metallic nickel toughened ceramic material.The gold that this research uses
It is the beta-silicon nitride powder using the cladding nickel of chemical plating to belong to nickel-ceramic composite powder.And important technology in this research
One of difficult point and research contents.Preparing metal-ceramic composite powder at present mainly has mechanical mixture, high-energy ball milling, self propagating high temperature to close
Into, reaction in-situ, sol-gel, vapour deposition, chemical plating several method.It is for metallic cover ceramic powder using chemically plating
Simply on powder granule surface the oxidation of generation metal simple-substance occurs for the technology that the beginning of this century rises, chemical plating principle also very
Original reaction, but its process control procedure is more complicated.Have metallic cover oxide ceramic powder body and carbide ceramics powder at present
The composite powder of body, the rare report of silicon nitride powder.Because different powder surface functional groups has bigger difference, in chemical plating fluid
The different influence of meeting is produced to the dynamic process of chemical plating, therefore for each ceramic powder, it is necessary to grope different changes
Learn depositing process parameter.Test of many times is passed through in this research, has found out a set of efficient suitable beta-silicon nitride powder cladding metal layer
Chemical plating process, has successfully prepared nickel coated silicon nitride powder at present, and the metal nickel content of cladding can control as needed
In the range of 1-60wt%.The content for coating metal is extremely important to the intensity for preparing metal-silicon nitride ceramic composite.
Hunan University of Technology it is silver-colored it is sharp it is bright《Central South University's journal》Paper " Fe coated Sis on (from section's version)3N4Metal
Ceramic phase thermodynamics of reactions is analyzed " prepare Fe coating alphas-Si using non-homogeneous phase deposition thermal reduction3N4Composite powder, and have studied
Its normal pressure-sintered interfacial reaction characteristic.
The Master's thesis " Study on Preparation of nickel coated beta-silicon nitride powder " of Chinese Marine University Liu Zhong virtues is using chemistry
Depositing process, but what he utilized is that nickel chloride is nickel source, and hydrazine hydrate is reducing agent, and palladium bichloride is activator.And his research is
Nickel coated silicon nitride powder is prepared for, it is not studied and is used for sintering and prepare nickel-silicon nitride composite material.
Above-mentioned two documents are prepared in nickel-silicon nitride composite powder technology for the existing of representative, the sharp bright research of silver and sheet
Invention has the difference of essence, he prepares iron cladding beta-silicon nitride powder using heterogeneous precipitation thermal reduction, and the present invention uses
Chemical plating process prepares nickel coated silicon nitride composite powder.Though the research of Liu Zhong virtues is to use chemical plating process, have with the present invention
Many significant differences.The selection of the compositional system and sensitizer of chemical plating fluid is determining for chemical plating success or not in chemical plating process
Qualitative link, different chemical plating fluids and sensitizer have conclusive influence to the quality of coating.The chemical plating that Liu Zhongfang is used
Liquid is nickel chloride and hydrazine hydrate system, for sensitizer uses palladium bichloride, hydrazine hydrate and palladium bichloride compared with sodium hypophosphite and silver nitrate
Belong to reagent costly.This and the nickel sulfate, the sodium hypophosphite plating solution that are used in the present invention, and silver nitrate are thin for the technique of sensitizer
Section has great difference；And chemical plating fluid is nickel source nickel chloride in the technique of Liu Zhongfang and reducing agent hydrazine hydrate is in advance directly
The mixing mother liquor mixed, when redox reaction so occurs on beta-silicon nitride powder surface, the generating process ratio of nickel layer
Compared with concentration, phenomenon in uneven thickness occurs in the nickel layer of cladding；Reducing agent sodium hypophosphite uses what is be slowly added dropwise in the present invention
Form, can so control the slow generation of redox reaction, that is, the slow generation of nickel layer, this is uniform to preparing thickness
Nickel layer have very important significance.Furthermore it is not directed in the research of Liu Zhongfang and is sintered using the nickel coated silicon nitride powder of its preparation
The problem of nickel silicon nitride composite material.In sintering because nickel to be solved the problems such as being stabilized, it is necessary to from formula design and burn
Determining etc. into system carries out many experiments, can just resolve the problem that is stabilized of metallic nickel, this research is to nickel nitridation
Silicon powder sintering has made intensive studies, and makes and comes relatively preferable formula system and calcining system.
The content of the invention
It is an object of the invention to provide a kind of technique for preparing metallic nickel-silicon nitride composite material.Its technical solution is：
(1) beta-silicon nitride powder for being coated with metal nickel layer is first prepared with chemical plating process, by controlling sensitization in chemical plating process, activating
Processing mode, reducing agent, plating solution composition and the technological parameter such as concentration and electroless plating time control nickel layer thick；(2) will cladding
The silicon nitride composite powder of metal nickel layer and the extra-fine nickel powder of 3-10wt%, 1-3wt.% activity powdered carbons, scattered Jie is with ethanol
Matter, abrasive media is done with a diameter of 2-3mm silicon nitrides bead, is dried in nylon tank after quick ball milling 30min, mixing is made
The usage percentage of powder, wherein extra-fine nickel powder and active powdered carbon is all in accordance with the silicon nitride composite powder of cladding metal nickel layer used
Dosage calculates；(3) by the mixed powder compressing bulks of cold isostatic press 100MPa；(4) sample that will be suppressed, is put into more work(
Vacuum pressed sinters in energy sintering furnace, pressure 25MPa；1600 DEG C of sintering schedule, 2h；Vacuum≤1.0 × 10-2Pa；(5) stove is treated
To after room temperature after warm natural cooling, you can obtain metallic nickel-silicon nitride composite material.
The technique for preparing nickel-silicon nitride composite material, the specific technical process in step (1) are：Will be average
Particle diameter is that 0.3-1 μm of silicon nitride original powder is put into HNO36-10h, wherein HNO are stirred in solution3The body of concentrated nitric acid and water in solution
Product ratio 1:3, concentrated nitric acid used is the nitric acid that commercial available quality concentration is 65%, this process is roughening；Silicon nitride after roughening
Powder is separated, and is put into SnCl2And HNO3Mixed solution in, 50 DEG C of stirring 6h, in mixed solution, SnCl2Concentration is 15-
30g/l, concentrated nitric acid dosage are 30-45ml/l, this process is sensitization；Beta-silicon nitride powder after being sensitized is separated, and is put into
AgNO3And HNO3Mixed solution in, be stirred at room temperature 6h, in mixed solution, AgNO3Concentration is 0.5-2g/l, and concentrated nitric acid dosage is
150-250ml/l, this process is activation；Beta-silicon nitride powder after activation is separated, and it is 50-80g/l's to be put into concentration
NiSO4In solution, it is 11 to adjust its pH with NaOH, buffer solution, and buffer solution is acetic acid-sodium acetate mixed solution, wherein second
Acid, sodium acetate concentration are 20-30g/l, stirring at normal temperature 0.5h, and it is 30-60g/l's that a certain amount of concentration is then added dropwise into system
NaH2PO2Solution, wherein NaH2PO2Solution usage need to be calculated according to added silicon nitride original powder amount, be stirred when being added dropwise, during dropwise addition
Between 1h or so, during system temperature control continue to stir 6-10h at 70 DEG C at 70 DEG C or so, after dripping, this process
Chemical plating, the beta-silicon nitride powder after having plated are separated, you can obtain being coated with the beta-silicon nitride powder of metal nickel layer；
The preparation process for preparing metallic nickel-silicon nitride composite material, needs in step (2) to add 3-10wt%'s
The usage percentage of extra-fine nickel powder and 1-3wt.% activity powdered carbons, wherein extra-fine nickel powder and active powdered carbon is all in accordance with cladding gold used
The dosage for belonging to the silicon nitride composite powder of nickel layer calculates；
The preparation process for preparing metallic nickel-silicon nitride composite material, the general basis of sintering temperature in step (4)
Beta-silicon nitride powder surface coats the species of metal to determine；The sintering schedule for determining nickel-silicon nitride ceramic material is one multiple
Miscellaneous process is, it is necessary to carry out multiple sintering test to determine.Fusing point such as nickel is 1453 DEG C, but if sintering at such a temperature,
Nickel is easy to generate NiSi, NiSi with silicon nitride2, at this time, NiSi, NiSi2Not yet largely reacted with C, in crystal boundary mainly
NiSi、NiSi2Phase, metallic nickel keep less, cause the intensity of sample not high；And when temperature rises to more than 1600 DEG C, NiSi,
NiSi2Start largely to generate Ni and SiC with the C of addition, at this time, because keeping higher vacuum, the guarantor that nickel can just be stablized in stove
Presence is held, greatly improves the intensity of sample.
The technological principle of the present invention：The Toughening Mechanism of cermet has been used for reference in this research, proposes to extend using with good
Property metallic nickel be used as combine mutually carry out toughening silicon nitride ceramics, first by beta-silicon nitride powder surface coat one layer of metal nickel layer, together
When the incorporation of the metallic Ni particles of certain mass percent is coated with the nitridation powder material of nickel layer, it is suitable true by selecting
Empty hot pressing calcining system, makes metallic nickel exist in the holding that can stablize after burning till between silicon nitride particle, is formed to have and necessarily prolonged
The metallic grain boundaries of malleability, the toughness of material is improved using the mechanism of the plastic deformation absorption energy to failure of metal.It is prepared out
What is used at low ambient temperatures has excellent impact resistance can be with nickel-silicon nitride composite material of high-strength wearable.
Embodiment
Embodiment 1：
Step 1：Nickel coated silicon nitride powder is prepared with chemical plating process.First with certain density HNO3Solution (concentrated nitric acid:Steam
Distilled water is 1:3) average grain diameter is roughened 10h for 0.5 μm of silicon nitride original powder；It is 15g/l's in concentration by the original powder after roughening
SnCl2With dilute HNO3Mixed solution (concentrated nitric acid dosage is 40ml/l) in sensitization 6h；Then the silicon nitride powder after sensitization is put into
Concentration is 0.6g/lAgNO3And HNO3Mixed solution (concentrated nitric acid dosage is 150ml/l) in activation 6h；Finally by after activation
It is 50g/l NiSO that silicon nitride powder, which is put into by concentration,4In, it is 11 to adjust pH, and the NaH that concentration is 35g/l is slowly added dropwise2PO2Solution,
And when stirring 6 is small under 70 DEG C of heating water baths, powder is finally filtered out into drying, you can obtain the silicon nitride of cladding certain thickness nickel layer
Powder.
Step 2：The a certain amount of above-mentioned nitridation silica fine powder for being coated with nickel layer is weighed, according still further to the silicon nitride powder of cladding nickel used
Gross mass calculates, and weighs the nickel powder and 1wt% activated carbon powders of 3wt%.
Step 3：Silicon nitride powder, metal nickel powder and the activated carbon powder of the cladding nickel weighed up are put into nylon ball grinder, used
Ethanol does decentralized medium, and 2-3mm silicon nitride balls after quick ball milling 30min, are dried to obtain mixed powder as ball-milling medium.
Step 4：By mixed powder cold isostatic press, the briquet under 100MPa；(3) the block sample that will be suppressed,
It is put into vacuum pressed in multifunctional sintering furnace to sinter, pressure 25MPa；1600 DEG C, 2h of sintering schedule, vacuum≤1.0 × 10- 2Pa。
Step 5：To after room temperature after furnace temperature natural cooling, you can obtain nickel-silicon nitride composite material.
Embodiment 2：
Step 1：Nickel coated silicon nitride powder is prepared with chemical plating process.First with certain density HNO3Solution (concentrated nitric acid:Steam
Distilled water is 1:3) average grain diameter is roughened 10h for 0.5 μm of silicon nitride original powder；It is 20g/l's in concentration by the original powder after roughening
SnCl2With dilute HNO3Mixed solution (concentrated nitric acid dosage is 40ml/l) in sensitization 6h；Then the silicon nitride powder after sensitization is put into
Concentration is 1.0g/lAgNO3And HNO3Mixed solution (concentrated nitric acid dosage is 150ml/l) in activation 6h；Finally by after activation
It is 60g/l NiSO that silicon nitride powder, which is put into by concentration,4In, it is 11 to adjust pH, and the NaH that concentration is 45g/l is slowly added dropwise2PO2Solution,
And when stirring 8 is small under 70 DEG C of heating water baths, powder is finally filtered out into drying, you can obtain the silicon nitride of cladding certain thickness nickel layer
Powder.
Step 2：The a certain amount of above-mentioned nitridation silica fine powder for being coated with nickel layer is weighed, according still further to the silicon nitride powder of cladding nickel used
Gross mass calculates, and weighs the nickel powder and 2wt% activated carbon powders of 5wt%.
Step 3：Silicon nitride powder, metal nickel powder and the activated carbon powder of the cladding nickel weighed up are put into nylon ball grinder, used
Ethanol does decentralized medium, and 2-3mm silicon nitride balls after quick ball milling 30min, are dried to obtain mixed powder as ball-milling medium.
Step 4：By mixed powder cold isostatic press, the briquet under 100MPa；(3) the block sample that will be suppressed,
It is put into vacuum pressed in multifunctional sintering furnace to sinter, pressure 25MPa；1600 DEG C, 2h of sintering schedule, vacuum≤1.0 × 10- 2Pa。
Step 5：To after room temperature after furnace temperature natural cooling, you can obtain nickel-silicon nitride composite material.
Embodiment 3：
Step 1：Nickel coated silicon nitride powder is prepared with chemical plating process.First with certain density HNO3Solution (concentrated nitric acid:Steam
Distilled water is 1:3) average grain diameter is roughened 10h for 0.5 μm of silicon nitride original powder；It is 25g/l's in concentration by the original powder after roughening
SnCl2With dilute HNO3Mixed solution (concentrated nitric acid dosage is 40ml/l) in sensitization 6h；Then the silicon nitride powder after sensitization is put into
Concentration is 1.5g/lAgNO3And HNO3Mixed solution (concentrated nitric acid dosage is 150ml/l) in activation 6h；Finally by after activation
It is 70g/l NiSO that silicon nitride powder, which is put into by concentration,4In, it is 11 to adjust pH, and the NaH that concentration is 50g/l is slowly added dropwise2PO2Solution,
And when stirring 10 is small under 70 DEG C of heating water baths, powder is finally filtered out into drying, you can obtain the nitridation of cladding certain thickness nickel layer
Silicon powder.
Step 2：The a certain amount of above-mentioned nitridation silica fine powder for being coated with nickel layer is weighed, according still further to the silicon nitride powder of cladding nickel used
Gross mass calculates, and weighs the nickel powder and 3wt% activated carbon powders of 7wt%.
Step 3：Silicon nitride powder, metal nickel powder and the activated carbon powder of the cladding nickel weighed up are put into nylon ball grinder, used
Ethanol does decentralized medium, and 2-3mm silicon nitride balls after quick ball milling 30min, are dried to obtain mixed powder as ball-milling medium.
Step 4：By mixed powder cold isostatic press, the briquet under 100MPa；(3) the block sample that will be suppressed,
It is put into vacuum pressed in multifunctional sintering furnace to sinter, pressure 25MPa；1600 DEG C, 2h of sintering schedule, vacuum≤1.0 × 10- 2Pa。
Step 5：To after room temperature after furnace temperature natural cooling, you can obtain nickel-silicon nitride composite material.
Embodiment 4：
Step 1：Nickel coated silicon nitride powder is prepared with chemical plating process.First with certain density HNO3Solution (concentrated nitric acid:Steam
Distilled water is 1:3) average grain diameter is roughened 10h for 0.5 μm of silicon nitride original powder；It is 30g/l's in concentration by the original powder after roughening
SnCl2With dilute HNO3Mixed solution (concentrated nitric acid dosage is 40ml/l) in sensitization 6h；Then the silicon nitride powder after sensitization is put into
Concentration is 2g/lAgNO3And HNO3Mixed solution (concentrated nitric acid dosage is 150ml/l) in activation 6h；Finally by the nitrogen after activation
It is 80g/l NiSO that SiClx powder, which is put into by concentration,4In, it is 11 to adjust pH, and the NaH that concentration is 60g/l is slowly added dropwise2PO2Solution, and
When stirring 10 is small under 70 DEG C of heating water baths, powder is finally filtered out into drying, you can obtain the silicon nitride of cladding certain thickness nickel layer
Powder.
Step 2：The a certain amount of above-mentioned nitridation silica fine powder for being coated with nickel layer is weighed, according still further to the silicon nitride powder of cladding nickel used
Gross mass calculates, and weighs the nickel powder and 3wt% activated carbon powders of 10wt%.
Step 3：Silicon nitride powder, metal nickel powder and the activated carbon powder of the cladding nickel weighed up are put into nylon ball grinder, used
Ethanol does decentralized medium, and 2-3mm silicon nitride balls after quick ball milling 30min, are dried to obtain mixed powder as ball-milling medium.
Step 4：By mixed powder cold isostatic press, the briquet under 100MPa；(3) the block sample that will be suppressed,
It is put into vacuum pressed in multifunctional sintering furnace to sinter, pressure 25MPa；1600 DEG C, 2h of sintering schedule, vacuum≤1.0 × 10- 2Pa。
Step 5：To after room temperature after furnace temperature natural cooling, you can obtain nickel-silicon nitride composite material.
Claims (1)
1. a kind of preparation process of nickel-silicon nitride composite material, it is characterised in that using following steps：(1) chemical plating work is first used
Skill prepares the beta-silicon nitride powder for being coated with metal nickel layer；Specifically technical process is：By the silicon nitride that average grain diameter is 0.3-1 μm
Original powder is put into HNO36-10h, wherein HNO are stirred in solution3The volume ratio 1 of concentrated nitric acid and water in solution:3, concentrated nitric acid used is
Commercial available quality concentration is 65% nitric acid, this process is roughening；Beta-silicon nitride powder after roughening is separated, and is put into SnCl2
And HNO3Mixed solution in, 50 DEG C of stirring 6h, in mixed solution, SnCl2Concentration is 15-30g/l, and concentrated nitric acid dosage is 30-
45ml/l, this process is sensitization；Beta-silicon nitride powder after being sensitized is separated, and is put into AgNO3And HNO3Mixed solution
In, it is stirred at room temperature 6h, in mixed solution, AgNO3Concentration is 0.5-2g/l, and concentrated nitric acid dosage is 150-250ml/l, this process
Cry activation；Beta-silicon nitride powder after activation is separated, and is put into the NiSO that concentration is 50-80g/l4In solution, with NaOH, buffering
It is 11 that solution, which adjusts its pH, and buffer solution is acetic acid-sodium acetate mixed solution, and wherein acetic acid, sodium acetate concentration is 20-30g/
L, stirring at normal temperature 0.5h, are then added dropwise the NaH that a certain amount of concentration is 30-60g/l into system2PO2Solution, wherein NaH2PO2It is molten
Liquid used in amounts is calculated according to added silicon nitride original powder amount, while be added dropwise while stir, time for adding 1h or so, during system temperature control
System continues stirring 6-10h, this process is chemical plating, the beta-silicon nitride powder after having plated at 70 DEG C or so at 70 DEG C after dripping
Separate, you can obtain being coated with the beta-silicon nitride powder of metal nickel layer；(2) silicon nitride composite powder of metal nickel layer will be coated
With the extra-fine nickel powder of 3-10wt.%, 1-3wt.% activity powdered carbons, decentralized medium is done with ethanol, small with a diameter of 2-3mm silicon nitrides
Ball does abrasive media, is dried in nylon tank after quick ball milling 30min, and mixed powder, wherein extra-fine nickel powder and active powdered carbon is made
Usage percentage all in accordance with it is used cladding metal nickel layer silicon nitride composite powder dosage calculate；(3) by mixed powder with cold
The compressing bulks of isostatic pressing machine 100MPa；(4) sample that will be suppressed, is put into vacuum pressed in multifunctional sintering furnace and sinters,
Pressure 25MPa；1600 DEG C of sintering schedule, 2h；Vacuum≤1.0 × 10-2Pa；(5) after furnace temperature cooled to room temperature, you can
Obtain metallic nickel-silicon nitride composite material.
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| CN109957739A (en) * | 2017-12-14 | 2019-07-02 | 宜兴安纳西智能机械设备有限公司 | A kind of battery conveying device inlet side frame material |
| 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 |
| CN113149677B (en) * | 2021-04-29 | 2022-11-22 | 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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