CN101195901A - Reaction spray coating metal ceramic composite powder and method for producing the same - Google Patents
Reaction spray coating metal ceramic composite powder and method for producing the same Download PDFInfo
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- CN101195901A CN101195901A CNA2007101718724A CN200710171872A CN101195901A CN 101195901 A CN101195901 A CN 101195901A CN A2007101718724 A CNA2007101718724 A CN A2007101718724A CN 200710171872 A CN200710171872 A CN 200710171872A CN 101195901 A CN101195901 A CN 101195901A
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Abstract
The invention provides reaction metal spraying ceramic composite powder and the preparation method thereof, which comprises the following steps: firstly, metal and ceramic powder are mixed according to the proportion, and then put into a ball grinder to be ground, the ball material ratio is 2:1 to 3:1, ethanol is added to wet the powder fully, and the ball grinding is operated; secondly, the powder which is mixed evenly is dried; thirdly, adhesion agent is added into the compound powder, fully mixed and put on a tablet pressing machine to press; fourthly, the pressed blocks are put into a vacuum carbon tube furnace, heated, thermally insulated and then cooled; fifthly, the compound powder after being sintered is crashed and ball-ground, and the power which is required is screened out. The weight percentage of the components of the obtained composite powder is as follows: 63-77 percent of Ti powder, 17-33 percent of B4C, and 2-6 percent of bonding agent. The components of the powder of the invention are mixed, the bonding is good, the fluidity is good, and the full operation of the reaction in the spray coating process can be guaranteed to prepare ceramic composite coating with high performance.
Description
Technical field
The present invention relates to a kind of preparation method of technical field of cermet material, specifically is a kind of reaction spray coating metal ceramic composite powder and preparation method thereof.
Background technology
Reactive spray is meant self-propagating reaction and hot-spraying techniques is combined, utilize the reaction heat promotion spraying particle of self-propagating reaction and the fusing of product particle, thereby can obtain dystectic pottery or intermetallic compound coating that ordinary method is difficult to prepare, thereby can realize low cost, high-effect the high performance ceramic base coating for preparing.At present, occurred technology such as SHS electric arc spraying, SHS plasma spraying, thermal explosion reactive spray, coating relates to systems such as Ti-C, Ti-B, Ti-N, Mo-Si, Ni-Al, Ti-B-N.Owing to can utilize the heat of self-propagating reaction, can realize low power spraying high-melting-point ceramic coating, and coating and matrix bond excellence, even do not apply prime coat, coating and matrix are still in conjunction with firm, and coating can reach very high thickness.Yet, when being metal and pottery, because the difference of aspects such as the density of metal and pottery, granularity for the reactive spray raw material, metal and ceramics powder are directly sprayed after the mixing, the spraying reaction can't be carried out often, even formed needed coating, the combination of coating and matrix is also very poor.
Find that through literature search Chinese patent publication number CN1370852A has carried out mechanical reunion processing to the metal-ceramic composite powder of thermite reaction, has obtained FeAl-Al to prior art
2O
3-FeAl
2O
4Coating.The preparation method of composite powder mixes after drying with composite powder in this patent, and adding additives fully stirs, then oven dry, fragmentation.This method is simple, but the intensity of the composite powder of preparation is relatively poor.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art, a kind of reaction spray coating metal ceramic composite powder and preparation method thereof is provided, make it solve that sintering metal reacts inadequate problem in reactive spray process, to realize the thorough mixing between metal powder and ceramics powder, the preparation method is simple, the good fluidity of composite powder can satisfy the needs that subsequent reactions sprays.
The present invention is achieved by the following technical solutions:
Reaction spray coating metal ceramic composite powder involved in the present invention contains in the spraying raw material and adopts metal, two kinds of different powder of pottery, between metal and the pottery self-propagating reaction can take place.The component and the weight percent content thereof of reaction spray coating metal ceramic composite powder are as follows:
Ti powder 63-77%
B
4C powder 17%-33%
Described Ti powder degree is-200 orders～+ 325 orders.
Described B
4The C powder is a chemical pure, and granularity is 280 orders.
Described binding agent adopts polyvinyl alcohol (PVA), and its concentration (weight ratio) is 7%.
The preparation method of reaction spray coating metal ceramic composite powder involved in the present invention, be after metal, ceramic powder are mixed, the pre-reaction sintering takes place under low oxygen pressure behind the briquetting, the broken preparation method who forms the composite powder of good fluidity, its sintering temperature is controlled at below the temperature of powder generation self-propagating reaction.This method is particularly suitable for the preparation feedback dusty spray.
Aforesaid method of the present invention may further comprise the steps:
(1) metal, ceramic powder are proportionally mixed after, put into ball mill and carry out ball milling, ratio of grinding media to material is 2: 1～3: 1, adds ethanol with powder complete wetting, ball milling;
(2) with the powder for drying that mixes;
(3) binding agent of adding 2%-6% in composite powder, thorough mixing is put into compressing tablet on the tabletting machine:
(4) piece that will press is put in the vacuum carbon tube furnace, is heated to 800 ℃-1000 ℃, the insulation postcooling;
(5) with the composite powder fragmentation behind the sintering, ball milling filters out required powder.
In the step (1), described ball mill, its rotating speed are 580rpm; Described ball milling, its time is 10h-24h.
In the step (2), described drying, its temperature are 50 ℃.
In the step (3), describedly be put into compressing tablet on the tabletting machine, its pressure is 15MPa～20MPa, and the time is 10min.
In the step (4), described vacuum carbon tube furnace, its vacuum tightness remains on 10
-5Pa; Described insulation, its time is 1h-3h.
In the step (5), described screening is meant to filter out the powder of diameter for-50 μ m.
Compared with prior art, characteristics of the present invention are: metal-ceramic composite powder end composition is even, can guarantee fully carrying out of self-propagating reaction in the reactive spray process; Pre-reaction has taken place in composite powder after vacuum sintering, between metal and pottery mutual diffusion has taken place, mostly be irregularly shaped after the fragmentation, what have is subsphaeroidal, intensity can reach more than 2-3 times of mechanical agglomeration process intensity, is suitable for various hot-spraying techniqueies such as plasma spraying, detonation flame spraying.Adopt the metal-ceramic composite powder end of the present invention's preparation, in spraying with powder feeding N
2React, can prepare Ti-B-N base coating, this coating and matrix bond excellence be not even spray the thickness that yet can reach nearly 400 μ m under the situation of prime coat.
Description of drawings
Fig. 1 is the XRD analysis figure as a result of starting powder;
Fig. 2 is the composite powder XRD analysis figure as a result of preparation;
Fig. 3 is the composite powder SEM shape appearance figure of preparation;
Fig. 4 is the cross section shape appearance figure of the compound coating of preparation;
Fig. 5 is the XRD analysis figure as a result of the compound coating of preparation.
Embodiment
Below in conjunction with accompanying drawing embodiments of the invention are elaborated: present embodiment is being to implement under the prerequisite with the technical solution of the present invention, provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
Embodiment 1: reactive spray prepares the metal/ceramic compound coating on the Q235 steel
1. prepare the metal/ceramic composite powder
(1) 142g titanium valve and 54g boron carbide powder are put into planetary ball mill, ratio of grinding media to material is 2: 1, adds an amount of ethanol, and rotating speed is 580rpm, mixes 10h, to mixing;
(2) with the powder that stirs drying in oven at 50 ℃;
(3) polyvinyl alcohol adhesive of adding 4g in composite powder, thorough mixing is put into compressing tablet on the tabletting machine, and pressure is 15MPa, and the time is 10min:
(4) piece that will press is put in the vacuum carbon tube furnace, is heated to 900 ℃, and vacuum tightness remains on 10
-5Pa, insulation 1h postcooling;
(5) with the composite powder fragmentation behind the sintering, ball milling filters out the powder of diameter for-50 μ m.
2. reaction and plasma spraying prepares the metal/ceramic compound coating
(1) in the alligatoring on emery wheel of Q235 steel surface, exposes fresh metallic surface;
(2) the above-mentioned composite powder of 100g is packed in the powder feeder;
(3) connect the housing power supply;
(4) send argon gas, send into hydrogen simultaneously, the control arc power is 30KW, and the spray gun distance is 100mm, and the powder feeding nitrogen flow is 5L/min, at the direct metallize/ceramic composite coating in Q235 steel surface.
After testing:
1. composite granule
The XRD analysis of the composite granule after starting powder and the processing is shown in Fig. 1-2, and starting powder is made up of titanium and norbide, and Ti partly reacts in the composite powder of preparation, has generated TiC and TiB2.SEM pattern such as Fig. 3 of the composite granule of preparation show that the composite granule great majority are irregularly shaped, and part is spherical, and size is at 2-10 μ m.
2. coating
The cross section pattern of the coating of plasma spraying composite granule preparation and XRD such as Fig. 4-5 show.In Q235 steel collective, generated TiN-TiB
2Compound coating, even under the situation that does not spray prime coat, coating and matrix bond are good, and the nearly 400 μ m of coat-thickness, average microhardness reaches 1328.5HV
0.1
Embodiment 2:
1. prepare the metal/ceramic composite powder
(1) 126g titanium valve, 66g boron carbide powder are put into planetary ball mill, ratio of grinding media to material is 2.5: 1, adds the ethanol wet-milling, and rotating speed is 580rpm, mixes 17h, to mixing;
(2) with the powder that stirs drying in oven at 50 ℃;
(3) polyvinyl alcohol adhesive of adding 8g in composite powder, thorough mixing is put into compressing tablet on the tabletting machine, and pressure is 18MPa, and the time is 10min:
(4) piece that will press is put in the vacuum carbon tube furnace, is heated to 800 ℃, and vacuum tightness remains on 10
-5Pa, insulation 3h postcooling;
(5) with the composite powder fragmentation behind the sintering, ball milling filters out the powder of diameter for-50 μ m.
2. reaction and plasma spraying prepares the metal/ceramic compound coating
(1) in the alligatoring on emery wheel of Q235 steel surface, exposes fresh metallic surface;
(2) connect the housing power supply;
(3) send argon gas, send into hydrogen simultaneously, the control arc power is 24.5KW, and the spray gun distance is 120mm, and the powder feeding nitrogen flow is 3L/min, at Q235 steel surface spraying Ni bag Al prime coat;
(4) regulating arc power is 30KW, and the spray gun distance is 100mm, and the powder feeding gas flow is 5L/min, metallize/ceramic composite coating.
After testing: formed the Cr-Ti-N-B compound coating on the Q235 steel matrix, thickness reaches 700 μ m (comprising prime coat 150 μ m), and good with matrix bond, the coating average microhardness reaches 1267.8HV
0.1
Embodiment 3:
1. prepare the metal/ceramic composite powder
(1) 154g titanium valve, 34g boron carbide powder are put into planetary ball mill, ratio of grinding media to material is 3: 1, adds an amount of ethanol, and rotating speed is 580rpm, mixes 24h, to mixing;
(2) with the powder that stirs drying in oven at 50 ℃;
(3) polyvinyl alcohol adhesive of adding 12g in composite powder, thorough mixing is put into compressing tablet on the tabletting machine, and pressure is 20MPa, and the time is 10min:
(4) piece that will press is put in the vacuum carbon tube furnace, is heated to 1000 ℃, and vacuum tightness remains on 10
-5Pa, insulation 2h postcooling;
(5) with the composite powder fragmentation behind the sintering, ball milling filters out the powder of diameter for-50 μ m.
2. reaction and plasma spraying prepares the metal/ceramic compound coating
Its preparation flow is with embodiment 2
3. after testing: formed the Co-Ti-N-B compound coating on the Q235 steel matrix, thickness reaches 600 μ m (comprising prime coat 120 μ m), and good with matrix bond, the coating average microhardness reaches 1287.8HV
0.1
Claims (10)
1. a reaction spray coating metal ceramic composite powder is characterized in that, component and weight percent content thereof are as follows: Ti powder: 63%-77%, B
4C powder: 17%-33%, binding agent: 2%-6%.
2. reaction spray coating metal ceramic composite powder according to claim 1 is characterized in that, described Ti powder degree is-200 orders～+ 325 orders.
3. reaction spray coating metal ceramic composite powder according to claim 1 is characterized in that, described B
4The C powder is a chemical pure, and granularity is 280 orders.
4. reaction spray coating metal ceramic composite powder according to claim 1 is characterized in that, described binding agent adopts polyvinyl alcohol, and its weight ratio concentration is 7%.
5. the preparation method of a reaction spray coating metal ceramic composite powder as claimed in claim 1 is characterized in that, may further comprise the steps:
(1) metal, ceramic powder are proportionally mixed after, put into ball mill and carry out ball milling, ratio of grinding media to material is 2: 1～3: 1, adds ethanol with powder complete wetting, ball milling;
(2) with the powder for drying that mixes;
(3) binding agent of adding 2%-6% in composite powder, thorough mixing is put into compressing tablet on the tabletting machine:
(4) piece that will press is put in the vacuum carbon tube furnace, is heated to 800 ℃-1000 ℃, the insulation postcooling;
(5) with the composite powder fragmentation behind the sintering, ball milling filters out required powder.
6. the preparation method of reaction spray coating metal ceramic composite powder according to claim 1 is characterized in that, in the step (1), described ball mill, its rotating speed are 580rpm; Described ball milling, its time is 10h-24h.
7. according to the preparation method of claim 1 or 6 described reaction spray coating metal ceramic composite powders, it is characterized in that in the step (2), described drying, its temperature are 50 ℃.
8. the preparation method of reaction spray coating metal ceramic composite powder according to claim 1 is characterized in that, in the step (3), describedly is put into compressing tablet on the tabletting machine, and its pressure is 15MPa-20MPa, and the time is 10min.
9. the preparation method of reaction spray coating metal ceramic composite powder according to claim 1 is characterized in that, in the step (4), and described vacuum carbon tube furnace, its vacuum tightness remains on 10
-5Pa; Described insulation, its time is 1h-3h.
10. the preparation method of reaction spray coating metal ceramic composite powder according to claim 1 is characterized in that, in the step (5), described screening is meant to filter out the powder of diameter for-50 μ m.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102277549A (en) * | 2011-08-11 | 2011-12-14 | 江阴东大新材料研究院 | Self-propagation reaction spraying method for metal ceramic rod |
| CN102925890A (en) * | 2012-10-26 | 2013-02-13 | 山东大学 | Preparation method for corrosion-resistant coating of nickel-aluminum based intermetallic compound |
| CN104032253A (en) * | 2014-06-19 | 2014-09-10 | 河北科技大学 | Ti-B-C-N ceramic coating and preparation method thereof |
| CN104057095A (en) * | 2014-06-25 | 2014-09-24 | 北京科技大学 | Production line for low-oxygen-content hard alloy mixture and production technology thereof |
| CN104213067A (en) * | 2014-09-25 | 2014-12-17 | 上海交通大学 | Method for coating high-temperature corrosion and wear resistant coating layer on surface of steel material |
| CN104493168A (en) * | 2014-12-27 | 2015-04-08 | 株洲茂翔硬质合金有限公司 | Preparation method for metal ceramic products |
| CN106270493A (en) * | 2016-08-03 | 2017-01-04 | 成都锦钛精工科技有限公司 | A kind of ceramic metal composite alloy spherical powder and preparation method thereof |
| CN110453170A (en) * | 2019-09-10 | 2019-11-15 | 常州大学 | A method of compact oxidation layer is formed in Fe-Cr-Si system alloy surface |
| CN112077325A (en) * | 2020-09-14 | 2020-12-15 | 明德新材料科技(浙江)股份有限公司 | Preparation method of metal surface coating with strong weather resistance |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3804034A (en) * | 1972-05-09 | 1974-04-16 | Boride Prod Inc | Armor |
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2007
- 2007-12-06 CN CN200710171872A patent/CN100595314C/en not_active Expired - Fee Related
Cited By (19)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102277549A (en) * | 2011-08-11 | 2011-12-14 | 江阴东大新材料研究院 | Self-propagation reaction spraying method for metal ceramic rod |
| CN102925890A (en) * | 2012-10-26 | 2013-02-13 | 山东大学 | Preparation method for corrosion-resistant coating of nickel-aluminum based intermetallic compound |
| CN102925890B (en) * | 2012-10-26 | 2014-07-09 | 山东大学 | Preparation method for corrosion-resistant coating of nickel-aluminum based intermetallic compound |
| CN104032253A (en) * | 2014-06-19 | 2014-09-10 | 河北科技大学 | Ti-B-C-N ceramic coating and preparation method thereof |
| CN104032253B (en) * | 2014-06-19 | 2016-09-14 | 河北科技大学 | A kind of Ti-B-C-N ceramic coating and preparation method thereof |
| CN104057095A (en) * | 2014-06-25 | 2014-09-24 | 北京科技大学 | Production line for low-oxygen-content hard alloy mixture and production technology thereof |
| CN104213067A (en) * | 2014-09-25 | 2014-12-17 | 上海交通大学 | Method for coating high-temperature corrosion and wear resistant coating layer on surface of steel material |
| CN104493168A (en) * | 2014-12-27 | 2015-04-08 | 株洲茂翔硬质合金有限公司 | Preparation method for metal ceramic products |
| CN106270493A (en) * | 2016-08-03 | 2017-01-04 | 成都锦钛精工科技有限公司 | A kind of ceramic metal composite alloy spherical powder and preparation method thereof |
| CN108213411A (en) * | 2016-08-03 | 2018-06-29 | 成都锦钛精工科技有限公司 | Coating spraying and 3D printing cermet material based on TiCN-MxC-Co and preparation method thereof |
| CN108213410A (en) * | 2016-08-03 | 2018-06-29 | 成都锦钛精工科技有限公司 | Coating spraying and 3D printing cermet material based on (Ti, Me) CN-MxC-Co and preparation method thereof |
| CN108315628A (en) * | 2016-08-03 | 2018-07-24 | 成都锦钛精工科技有限公司 | Coating spraying and 3D printing cermet material based on (Ti, Me) CN-Co and preparation method thereof |
| CN106270493B (en) * | 2016-08-03 | 2020-06-30 | 成都锦钛精工科技有限公司 | Metal ceramic composite alloy spherical powder and preparation method thereof |
| CN108213411B (en) * | 2016-08-03 | 2020-08-25 | 成都锦钛精工科技有限公司 | Coating spraying and 3D printing cermet material based on TiCN-MxC-Co and preparation method thereof |
| CN108213410B (en) * | 2016-08-03 | 2020-09-08 | 成都锦钛精工科技有限公司 | Based on (Ti, Me) CN-MxC-Co coating spraying and 3D printing cermet material and preparation method thereof |
| CN110453170A (en) * | 2019-09-10 | 2019-11-15 | 常州大学 | A method of compact oxidation layer is formed in Fe-Cr-Si system alloy surface |
| CN110453170B (en) * | 2019-09-10 | 2021-03-23 | 常州大学 | Method for forming compact oxide layer on surface of Fe-Cr-Si series alloy |
| CN112077325A (en) * | 2020-09-14 | 2020-12-15 | 明德新材料科技(浙江)股份有限公司 | Preparation method of metal surface coating with strong weather resistance |
| CN112077325B (en) * | 2020-09-14 | 2022-12-20 | 明德新材料科技(浙江)股份有限公司 | Preparation method of metal surface coating with strong weather resistance |
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