CN106676309A - Preparation method for diamond material coated with molybdenum carbide on surface - Google Patents
Preparation method for diamond material coated with molybdenum carbide on surface Download PDFInfo
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- CN106676309A CN106676309A CN201710024448.0A CN201710024448A CN106676309A CN 106676309 A CN106676309 A CN 106676309A CN 201710024448 A CN201710024448 A CN 201710024448A CN 106676309 A CN106676309 A CN 106676309A
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- Prior art keywords
- diamond
- diamond particles
- boat
- deionized water
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
- C22C1/1005—Pretreatment of the non-metallic additives
- C22C1/101—Pretreatment of the non-metallic additives by coating
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C26/00—Alloys containing diamond or cubic or wurtzitic boron nitride, fullerenes or carbon nanotubes
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/0047—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents
- C22C32/0052—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents only carbides
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a preparation method for a diamond material coated with molybdenum carbide on the surface. The preparation method comprises the following steps: after surface cleaning and activation on diamond particles, mechanically and uniformly mixing the obtained diamond particles and molybdenum powder at a molar ratio of (5-10): 1 in an alcohol medium and putting the mixture in a boat, adding a mixed salt of sodium chloride and potassium chloride at a molar ratio of 1: 1 to cover the boat, putting the boat in a tubular furnace, raising the temperature to 1050-1150 DEG C at a rate of 5-10 DEG C/min in a high pure argon atmosphere, and preserving the temperature for 15-60 minutes; and after furnace cooling, taking out the boat, and repeatedly cleaning the boat with deionized water at 80-90 DEG C several times to remove the fused salt so as to obtain the diamond particles coated with Mo2C.
Description
Technical field
The present invention relates to a kind of Mo of diamond surface2C clads and preparation method thereof, belong to the preparation skill of composite
Art.
Background technology
Diamond reinforced metal-base composite material is considered as a kind of very promising electronic package material.Diamond
Interface cohesion between metallic matrix is the factor for influenceing composite overall thermal conductivity most critical.
Diamond reinforced metal-base composite material has a theoretical thermal conductivity very high, but due to metal and diamond it
Between wetability it is poor so that the interface resistance of composite is larger, limits its application on electronic component.In order to improve
Interface cohesion problem in diamond reinforced metal-base composite material, researcher has done the scientific experiment of many correlations, wherein
Modified Diamond is a kind of very effective method.The method of usual Modified Diamond includes vacuum evaporation deposition
Method, magnetron sputtering method, chemical vapour deposition technique, chemical plating, sol-gal process, diffusion method and molten-salt growth method etc., and be evaporated in vacuo
Sedimentation and magnetron sputtering method are all higher to equipment requirement；The technical process of chemical plating is complex, it is necessary to be sensitized through overactivation
Deng treatment；Sol-gal process has that cladding is imperfect；There is cladding problem of non-uniform in diffusion method；Simultaneously different strong carbonizations
The suitable cladding mode of thing formation element is also different.So, in order to improve the interface cohesion between diamond and metallic matrix, choosing
A kind of suitable cladding mode and carbide source material are selected, one layer strong carbon is equably coated in diamond surface
Compound, has great importance.
The content of the invention
Present invention aim at a kind of surface coated diamond preparation method of molybdenum carbide of offer, the advantage of the method
It is preparation process is simple, by Mo2C clads are evenly distributed in diamond surface, and are firmly combined with diamond.The present invention
It is achieved through the following technical solutions,
A kind of surface coated diamond preparation method of molybdenum carbide, comprises the following steps：
1) pre-treatment
After cleaning diamond surface, with 10~25% nitric acid 0.5~more than 1h of stirring and washing, then will with deionized water
Diamond particles are cleaned by ultrasonic 3~5 times, dried for standby；
2) molten-salt growth method prepares Mo2C clads
By step 1) in the diamond particles that obtain and molybdenum powder with mol ratio be (5~10):1 is mechanical mixed in alcoholic media
It is put into Noah's ark after closing uniformly, it is 1 to add mol ratio:1 sodium chloride and the salt-mixture of potassium chloride are covered, and are put into tube furnace
In, under high-purity argon gas atmosphere, 1050~1150 DEG C are risen to the speed of 5~10 DEG C/min, it is incubated 15~60min；It is cold with stove
But after, Noah's ark taking-up is cleared up repeatedly with 80~90 DEG C of deionized water and removes fused salt for several times, obtain being coated with Mo2The Buddha's warrior attendant of C
Stone particle.
The present invention has advantages below and effect：Preparation process is simple, it is reproducible.Resulting Mo2C clads are uniform
Be distributed in diamond surface, and be firmly combined with diamond；The Mo that molybdenum source is obtained with diamond reaction is done by molybdenum powder2C crystal grain
Size uniformity, and the thick Mo of 500~1000nm can be obtained by shortening the reaction time2C clads；The Mo of minimal thickness2C is coated
Layer is more beneficial for promoting the interface cohesion between diamond and metallic matrix, reduces interface resistance, and the composite for obtaining has
Thermal conductivity higher.The sub-micron clad can be commonly utilized in the surface of diamond particles it is modified on, reduce composite
Interface resistance, improve composite interface cohesion.
Brief description of the drawings
Fig. 1 is coated with Mo to be obtained in the embodiment of the present invention 1,2,32The stereoscan photograph of C layers of diamond particles.
Fig. 2 is obtained diamond@Mo for the embodiment of the present invention 12Stereoscan photograph (the back of the body after the polishing of C/Cu composites
Scattered electron picture).
Fig. 3 is obtained diamond@Mo for the embodiment of the present invention 32Stereoscan photograph (the back of the body after the polishing of C/Cu composites
Scattered electron picture).
Fig. 4 is obtained diamond@Mo for the embodiment of the present invention 12The stereoscan photograph that C/Cu composite material interfaces amplify.
Fig. 5 is that the embodiment of the present invention 1,3 is obtained diamond@Mo2The distribution map of C/Cu heat conductivities.
Specific embodiment
With reference to embodiment, the invention will be further described, and these embodiments are only intended to the explanation present invention, not
The limitation present invention.
Embodiment 1：
1) prepare 10% potassium hydroxide solution 100mL, weigh 15g diamond particles be put into potassium hydroxide solution in stir
Cleaning 0.5h is mixed, is cleaned by ultrasonic diamond particles in deionized water three times afterwards, prepare 20% salpeter solution 100mL,
Diamond particles are put into stirring and washing 0.5h in salpeter solution, then diamond particles are cleaned by ultrasonic three in deionized water
Time, be put into afterwards in 80 DEG C of baking oven dry it is stand-by.
2) molybdenum powder 12g and step 1 are weighed) in the diamond particles that the prepare together mechanical mixture in alcoholic media
2h, taking-up is put into Noah's ark, and it is 1 to add mol ratio:1 sodium chloride and the salt-mixture of potassium chloride are covered, and are put into tube furnace
In, under high-purity argon gas atmosphere, 1050 DEG C are risen to the speed of 5~10 DEG C/min, it is incubated 15min；After furnace cooling, by Noah's ark
Taking-up is cleared up more than 3 times and removes fused salt repeatedly with 90 DEG C of deionized water, after then powder is dried with mortar grinder it is abundant after
Sieving, the powder ultrasonic cleaning after sieving obtains being coated with Mo after drying2The diamond particles of C.
The Mo that said process is prepared2C cladding diamonds particle uses vacuum pressure with 60% volume fraction and copper
Power infiltration method is made diamond@Mo2C/Cu composites, thermal conductivity test is carried out to it, as a result sees Fig. 4.
Embodiment 2：
1) prepare 10% potassium hydroxide solution 100mL, weigh 15g diamond particles be put into potassium hydroxide solution in stir
Cleaning 0.5h is mixed, is cleaned by ultrasonic diamond particles in deionized water three times afterwards, prepare 20% salpeter solution 100mL,
Diamond particles are put into stirring and washing 0.5h in salpeter solution, then diamond particles are cleaned by ultrasonic three in deionized water
Time, be put into afterwards in 80 DEG C of baking oven dry it is stand-by.
2) molybdenum powder 12g and step 1 are weighed) in the diamond particles that the prepare together mechanical mixture in alcoholic media
2h, taking-up is put into Noah's ark, and it is 1 to add mol ratio:1 sodium chloride and the salt-mixture of potassium chloride are covered, and are put into tube furnace
In, under high-purity argon gas atmosphere, 1050 DEG C are risen to the speed of 5~10 DEG C/min, it is incubated 30min；After furnace cooling, by Noah's ark
Taking-up is cleared up more than 3 times and removes fused salt repeatedly with 90 DEG C of deionized water, after then powder is dried with mortar grinder it is abundant after
Sieving, the powder ultrasonic cleaning after sieving obtains being coated with Mo after drying2The diamond particles of C.
Embodiment 2：
1) prepare 10% potassium hydroxide solution 100mL, weigh 15g diamond particles be put into potassium hydroxide solution in stir
Cleaning 0.5h is mixed, is cleaned by ultrasonic diamond particles in deionized water three times afterwards, prepare 20% salpeter solution 100mL,
Diamond particles are put into stirring and washing 0.5h in salpeter solution, then diamond particles are cleaned by ultrasonic three in deionized water
Time, be put into afterwards in 80 DEG C of baking oven dry it is stand-by.
2) molybdenum powder 12g and step 1 are weighed) in the diamond particles that the prepare together mechanical mixture in alcoholic media
2h, taking-up is put into Noah's ark, and it is 1 to add mol ratio:1 sodium chloride and the salt-mixture of potassium chloride are covered, and are put into tube furnace
In, under high-purity argon gas atmosphere, 1050 DEG C are risen to the speed of 5~10 DEG C/min, it is incubated 60min；After furnace cooling, by Noah's ark
Taking-up is cleared up more than 3 times and removes fused salt repeatedly with 90 DEG C of deionized water, after then powder is dried with mortar grinder it is abundant after
Sieving, the powder ultrasonic cleaning after sieving obtains being coated with Mo after drying2The diamond particles of C.
The Mo that said process is prepared2C cladding diamonds particle uses vacuum pressure with 60% volume fraction and copper
Power infiltration method is made diamond@Mo2C/Cu composites, thermal conductivity test is carried out to it, as a result sees Fig. 4.
To sum up, technology path of the invention is as follows：
1) pre-treatment：The potassium hydroxide solution for taking 10%~25% is appropriate, and diamond particles are put into wherein stirring and washing
, be cleaned by ultrasonic diamond particles 3~5 times with deionized water, then use by 0.5~1h, it is therefore an objective to remove the greasy dirt of diamond surface
10~25% 0.5~1h of nitric acid stirring and washing, it is therefore an objective to remove the metal impurities and activation diamond of diamond surface, then
Diamond particles are cleaned by ultrasonic 3~5 times with deionized water, are dried in 80 DEG C of baking ovens stand-by.
2) molten-salt growth method prepares Mo2C clads
By step 1) in the diamond particles that obtain and molybdenum powder with mol ratio be (5~10):1 is mechanical mixed in alcoholic media
It is put into Noah's ark after closing uniformly, it is 1 to add mol ratio:1 sodium chloride and the salt-mixture of potassium chloride are covered, and are put into tube furnace
In, under high-purity argon gas atmosphere, 1050~1150 DEG C are risen to the speed of 5~10 DEG C/min, it is incubated 15~60min；It is cold with stove
But after, Noah's ark is taken out and is cleared up repeatedly with 80~90 DEG C of deionized water and is removed fused salt for several times, with grinding after then powder is dried
Sieving after alms bowl grinding fully, the powder ultrasonic cleaning after sieving obtains being coated with Mo after drying2The diamond particles of C.
Claims (1)
1. a kind of surface coated diamond preparation method of molybdenum carbide, comprises the following steps：
1) pre-treatment
After cleaning diamond surface, with 10~25% nitric acid 0.5~more than 1h of stirring and washing, then with deionized water by Buddha's warrior attendant
Stone particle is cleaned by ultrasonic 3~5 times, dried for standby；
2) molten-salt growth method prepares Mo2C clads
By step 1) in the diamond particles that obtain and molybdenum powder with mol ratio be (5~10):1 in alcoholic media mechanical mixture it is equal
It is put into Noah's ark after even, it is 1 to add mol ratio:1 sodium chloride and the salt-mixture of potassium chloride are covered, and are put into tube furnace,
Under high-purity argon gas atmosphere, 1050~1150 DEG C are risen to the speed of 5~10 DEG C/min, be incubated 15~60min；Furnace cooling
Afterwards, Noah's ark is taken out to be cleared up repeatedly with 80~90 DEG C of deionized water and removes fused salt for several times, obtain being coated with Mo2The diamond of C
Particle.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710024448.0A CN106676309A (en) | 2017-01-13 | 2017-01-13 | Preparation method for diamond material coated with molybdenum carbide on surface |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201710024448.0A CN106676309A (en) | 2017-01-13 | 2017-01-13 | Preparation method for diamond material coated with molybdenum carbide on surface |
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| CN106676309A true CN106676309A (en) | 2017-05-17 |
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| CN201710024448.0A Pending CN106676309A (en) | 2017-01-13 | 2017-01-13 | Preparation method for diamond material coated with molybdenum carbide on surface |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110878418A (en) * | 2018-09-06 | 2020-03-13 | 天津大学 | Self-supporting molybdenum carbide and preparation method and application thereof |
| CN114349001A (en) * | 2022-01-22 | 2022-04-15 | 河南厚德钻石科技有限公司 | Purification treatment method of diamond micro powder prepared by mechanical crushing method |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103388142A (en) * | 2013-07-29 | 2013-11-13 | 东南大学 | Method for plating tungsten on diamond surface |
| CN104962771A (en) * | 2015-05-25 | 2015-10-07 | 西安交通大学 | Directional porous SiC and diamond reinforced Al base composite material and preparation method thereof |
| CN105671542A (en) * | 2016-03-10 | 2016-06-15 | 江苏大学 | Diamond salt fusing and tungsten plating method |
-
2017
- 2017-01-13 CN CN201710024448.0A patent/CN106676309A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103388142A (en) * | 2013-07-29 | 2013-11-13 | 东南大学 | Method for plating tungsten on diamond surface |
| CN104962771A (en) * | 2015-05-25 | 2015-10-07 | 西安交通大学 | Directional porous SiC and diamond reinforced Al base composite material and preparation method thereof |
| CN105671542A (en) * | 2016-03-10 | 2016-06-15 | 江苏大学 | Diamond salt fusing and tungsten plating method |
Non-Patent Citations (1)
| Title |
|---|
| 马松地等: ""Mo2C coating on diamond：Different effects on thermal conductivity of diamond/Al and diamond/Cu composites"", 《APPLIED SURFACE SCIENCE》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110878418A (en) * | 2018-09-06 | 2020-03-13 | 天津大学 | Self-supporting molybdenum carbide and preparation method and application thereof |
| CN114349001A (en) * | 2022-01-22 | 2022-04-15 | 河南厚德钻石科技有限公司 | Purification treatment method of diamond micro powder prepared by mechanical crushing method |
| CN114349001B (en) * | 2022-01-22 | 2024-02-20 | 河南厚德钻石科技有限公司 | Purifying treatment method for diamond micropowder prepared by mechanical crushing method |
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