CN105236987A - Silicon carbide/molybdenum disulfide composite ceramic and preparation method thereof - Google Patents
Silicon carbide/molybdenum disulfide composite ceramic and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a silicon carbide/molybdenum disulfide composite ceramic and a preparation method thereof. The silicon carbide/molybdenum disulfide composite ceramic contains silicon carbide, graphite, molybdenum disulfide, water soluble resin, a plasticizer and a demolding agent, wherein the water soluble resin is selected from one or more of urea-formaldehyde resin, melamine formaldehyde resin, polyacrylic acid and polymethylacrylic acid, and the particle size of silicon carbide is 1-5 [mu]m. The silicon carbide/molybdenum disulfide composite ceramic has excellent wear resistance, heat resistance and mechanical properties, besides, the preparation method is simple in steps, and the raw materials are easy to obtain.
Description
Technical field
The present invention relates to composite ceramics, particularly, relate to a kind of silicon carbide/molybdenumdisulphide composite ceramics and preparation side thereof.
Background technology
Along with developing rapidly of science and technology, Brake Products is more and more high to the requirement of friction materials, except at a high speed, and the requirements at the higher level such as high temperature, outside the security in the bad working environments situations such as high pressure and comfortableness, also been proposed energy-conservation, environmental protection in recent years, clean.In China's the 12 five-year plan, propose clearly, the most important thing of the national economic development is energy-conservation, environmental protection, and steadily, the Scientific Outlook on Development continued, makes China develop into one in a short time and stablize, flourishing power.In 30 years of reform and opening-up, the friction industry of China is also the same with national all trades and professions, there is significant progress, be main from the asbestos friction material at the beginning of last century 80, develop into the semi-metal goods of the nineties gradually, 2000 later mixes and to optimize and nonmetal, and non-asbestos organic (NAO) goods are main.Successively release ceramic fibre brake component again in recent years, and move towards domestic and international market step by step.
Wherein, the visual field of people just come into by molybdenumdisulphide pottery, and molybdenumdisulphide pottery is obtained by the body material of molybdenumdisulphide and pottery, and molybdenumdisulphide pottery is mainly determined by the characteristic of molybdenumdisulphide as excellent friction materials.Molybdenumdisulphide is important solid lubricant, and under being specially adapted to High Temperature High Pressure, having following characteristics as during friction materials: antifriction during low temperature, increase during high temperature and rub, loss on ignition is little, volatile in friction materials.The effect that the molybdenumdisulphide that under low temperature, particle is less just can play anti-attrition because frictional coefficient is low; But once temperature raises, owing to there is the multipolymer of molybdenumdisulphide, molybdenum trisulfide and molybdic oxide in molybdenumdisulphide, the molybdenum trioxide particles in multipolymer expands along with intensification and just can serve the increasing effect of rubbing; In addition, molybdenumdisulphide covers the surface of friction materials, can protect other materials, prevents them oxidized, especially makes other materials difficult drop-off, and the power that attaches strengthens.Although molybdenumdisulphide pottery has served certain effect as friction materials, but the compatibility of molybdenumdisulphide and other components is not reach best in existing molybdenumdisulphide pottery, and then result in molybdenumdisulphide pottery and still wait to improve in thermotolerance and mechanical property.
Summary of the invention
The object of this invention is to provide a kind of silicon carbide/molybdenumdisulphide composite ceramics and preparation method thereof, this silicon carbide/molybdenumdisulphide composite ceramics has excellent wear resistance, thermotolerance and mechanical property, and meanwhile, this preparation method's step is simple, and raw material is easy to get.
To achieve these goals, the invention provides a kind of silicon carbide/molybdenumdisulphide composite ceramics, containing silicon carbide, graphite, molybdenumdisulphide, water soluble resin, softening agent and releasing agent;
Wherein, water soluble resin be selected from urea-formaldehyde resin, terpolycyantoamino-formaldehyde resin, polyacrylic acid and polymethyl acrylic acid one or more, the particle diameter of silicon carbide is 1-5 μm.
Invention further provides the preparation method of a kind of silicon carbide/molybdenumdisulphide composite ceramics, comprising:
1) silicon carbide, graphite, molybdenumdisulphide and water mixed and carry out grinding with obtained silicon carbide slurry;
2) water soluble resin mixed with silicon carbide slurry and carry out grinding with obtained first modified slurry;
3) softening agent mixed with the first modified slurry and carry out grinding with obtained second modified slurry;
4) releasing agent mixed with the second modified slurry and carry out grinding with obtained 3rd modified slurry;
5) the 3rd modified slurry is carried out drying with obtained silicon carbide/molybdenumdisulphide composite ceramics;
Wherein, water soluble resin be selected from urea-formaldehyde resin, terpolycyantoamino-formaldehyde resin, polyacrylic acid and polymethyl acrylic acid one or more, the particle diameter of silicon carbide is 1-5 μm.
Pass through technique scheme, preparation method provided by the invention, by silicon carbide, graphite, molybdenumdisulphide, softening agent and releasing agent being carried out powder mull in aqueous systems and then making each component can be compatible fully, obtains silicon carbide/molybdenumdisulphide composite ceramics finally by drying and moulding.This silicon carbide/molybdenumdisulphide composite ceramics has excellent wear resistance, thermotolerance and mechanical property under the synergy of silicon carbide, graphite, molybdenumdisulphide, softening agent and releasing agent, and then this composite ceramics can be used by further genralrlization in friction material field.
Other features and advantages of the present invention are described in detail in embodiment part subsequently.
Embodiment
Below the specific embodiment of the present invention is described in detail.Should be understood that, embodiment described herein, only for instruction and explanation of the present invention, is not limited to the present invention.
The invention provides a kind of silicon carbide/molybdenumdisulphide composite ceramics, containing silicon carbide, graphite, molybdenumdisulphide, water soluble resin, softening agent and releasing agent;
Wherein, water soluble resin be selected from urea-formaldehyde resin, terpolycyantoamino-formaldehyde resin, polyacrylic acid and polymethyl acrylic acid one or more, the particle diameter of silicon carbide is 1-5 μm.
In the present invention, the molecular weight of water soluble resin can be selected in wide scope, but in order to make this silicon carbide/molybdenumdisulphide composite ceramics have more excellent wear resistance, thermotolerance and mechanical property, preferably, the weight-average molecular weight of water soluble resin is 2000-20000.
In the present invention, the concrete kind of releasing agent and softening agent can be selected in wide scope, but in order to make this silicon carbide/molybdenumdisulphide composite ceramics, there is more excellent wear resistance, thermotolerance and mechanical property, preferably, releasing agent is selected from silicone oil, paraffin, polyethylene wax, talcum powder, mica.One or more in potter's clay and white clay, softening agent be selected from phthalic acid ester compounds, aliphatic dibasic acid ester compound, phosphate compounds, polyol ester compounds, benzene polyacid ester compound and citric acid ester type compound one or more.
In the present invention, the content of each component can be selected in wide scope, but in order to make this silicon carbide/molybdenumdisulphide composite ceramics, there is more excellent wear resistance, thermotolerance and mechanical property, preferably, relative to the silicon carbide of 100 weight parts, the content of graphite is 5-16 weight part, the content of molybdenumdisulphide is 11-26 weight part, the content of water soluble resin is 5-12 weight part, and the content of softening agent is 1-4 weight part, and the content of releasing agent is 0.5-1.4 weight part.
Invention further provides the preparation method of a kind of silicon carbide/molybdenumdisulphide composite ceramics, comprising:
1) silicon carbide, graphite, molybdenumdisulphide and water mixed and carry out grinding with obtained silicon carbide slurry;
2) water soluble resin mixed with silicon carbide slurry and carry out grinding with obtained first modified slurry;
3) softening agent mixed with the first modified slurry and carry out grinding with obtained second modified slurry;
4) releasing agent mixed with the second modified slurry and carry out grinding with obtained 3rd modified slurry;
5) the 3rd modified slurry is carried out drying with obtained silicon carbide/molybdenumdisulphide composite ceramics;
Wherein, water soluble resin be selected from urea-formaldehyde resin, terpolycyantoamino-formaldehyde resin, polyacrylic acid and polymethyl acrylic acid one or more, the particle diameter of silicon carbide is 1-5 μm.
In the preparation process in accordance with the present invention, the molecular weight of water soluble resin can be selected in wide scope, but in order to make the silicon carbide/molybdenumdisulphide composite ceramics obtained, there is more excellent wear resistance, thermotolerance and mechanical property, preferably, the weight-average molecular weight of water soluble resin is 2000-20000.
In the preparation process in accordance with the present invention, the concrete kind of releasing agent and softening agent can be selected in wide scope, but in order to make the silicon carbide/molybdenumdisulphide composite ceramics obtained, there is more excellent wear resistance, thermotolerance and mechanical property, preferably, releasing agent is selected from silicone oil, paraffin, polyethylene wax, talcum powder, mica.One or more in potter's clay and white clay, softening agent be selected from phthalic acid ester compounds, aliphatic dibasic acid ester compound, phosphate compounds, polyol ester compounds, benzene polyacid ester compound and citric acid ester type compound one or more.
In above-mentioned preparation method, the consumption of each component can be selected in wide scope, but in order to make the silicon carbide/molybdenumdisulphide composite ceramics obtained, there is more excellent wear resistance, thermotolerance and mechanical property, preferably, relative to the silicon carbide of 100 weight parts, the consumption of graphite is 5-16 weight part, the consumption of molybdenumdisulphide is 11-26 weight part, the consumption of water soluble resin is 5-12 weight part, the consumption of softening agent is 1-4 weight part, the consumption of releasing agent is 0.5-1.4 weight part, and the consumption of water is 99-170 weight part.
In above-mentioned preparation method, the solid content of silicon carbide slurry can be selected in wide scope, but in order to make the silicon carbide/molybdenumdisulphide composite ceramics obtained, there is more excellent wear resistance, thermotolerance and mechanical property, preferably, the solid content of silicon carbide slurry is 30 % by weight-40 % by weight.
In above-mentioned preparation method, grinding can take the lapping mode of this area any one routine, but in order to make the silicon carbide/molybdenumdisulphide composite ceramics obtained have more excellent wear resistance, thermotolerance and mechanical property, preferably, grinding is ball milling.Wherein, the milling time in each step also can be selected in wide scope, considers, more preferably, in step 1 from the performance of preparation efficiency and obtained composite ceramics) in, the time of grinding is 40-70min; In step 2) in, the time of grinding is 1-2h; In step 3) in, the time of grinding is 1-1.5h; In step 4) in, the time of grinding is 40-70min.
In above-mentioned preparation method, the dry drying mode can taking this area any one routine, but in order to make the silicon carbide/molybdenumdisulphide composite ceramics obtained have more excellent wear resistance, thermotolerance and mechanical property, preferably, in step 5) in, drying is spraying dry.Wherein, spray-dired actual conditions can be selected in wide scope, but in order to improve drying effect further, more preferably, spraying dry at least meets the following conditions: inlet temperature is 170-190 DEG C, and air outlet temperature is 120-140 DEG C, and time of drying is 40-80min.
Below will be described the present invention by embodiment.
Embodiment 1
1) silicon carbide (particle diameter is 3 μm), graphite, molybdenumdisulphide and water mixed according to the weight ratio of 100:10:18:140 and carry out ball milling 60min with obtained silicon carbide slurry (solid content is 35 % by weight);
2) mixed with silicon carbide slurry by water soluble resin (weight-average molecular weight is the urea-formaldehyde resin of 10000) and carry out ball milling 1.5h with obtained first modified slurry, wherein, in water soluble resin and silicon carbide slurry, the weight ratio of silicon carbide is 8:100;
3) mixed with the first modified slurry by softening agent (phthalic acid methyl ester) and carry out ball milling 1.2h with obtained second modified slurry, wherein, in softening agent and silicon carbide slurry, the weight ratio of silicon carbide is 2:100;
4) mixed with the second modified slurry by releasing agent (silicone oil) and carry out ball milling 60min with obtained 3rd modified slurry, wherein, in releasing agent and silicon carbide slurry, the weight ratio of silicon carbide is 1:100;
5) the 3rd modified slurry is carried out spraying dry 60min (inlet temperature is 180 DEG C, and air outlet temperature is 130 DEG C) with obtained silicon carbide/molybdenumdisulphide composite ceramics A1.
Embodiment 2
1) silicon carbide (particle diameter is 1 μm), graphite, molybdenumdisulphide and water mixed according to the weight ratio of 100:5:11:99 and carry out ball milling 40min with obtained silicon carbide slurry (solid content is 30 % by weight);
2) water soluble resin (weight-average molecular weight is the terpolycyantoamino-formaldehyde resin of 2000) mixed with silicon carbide slurry and carry out ball milling 1h with obtained first modified slurry, wherein, in water soluble resin and silicon carbide slurry, the weight ratio of silicon carbide is 5:100;
3) mixed with the first modified slurry by softening agent (tritolyl phosphate) and carry out ball milling 1h with obtained second modified slurry, wherein, in softening agent and silicon carbide slurry, the weight ratio of silicon carbide is 1:100;
4) mixed with the second modified slurry by releasing agent (polyethylene wax) and carry out ball milling 40min with obtained 3rd modified slurry, wherein, in releasing agent and silicon carbide slurry, the weight ratio of silicon carbide is 0.5:100;
5) the 3rd modified slurry is carried out spraying dry 40min (inlet temperature is 170 DEG C, and air outlet temperature is 120 DEG C) with obtained silicon carbide/molybdenumdisulphide composite ceramics A2.
Embodiment 3
1) silicon carbide (particle diameter is 5 μm), graphite, molybdenumdisulphide and water mixed according to the weight ratio of 100:16:26:170 and carry out ball milling 70min with obtained silicon carbide slurry (solid content is 40 % by weight);
2) water soluble resin (weight-average molecular weight is the polymethyl acrylic acid of 20000) mixed with silicon carbide slurry and carry out ball milling 2h with obtained first modified slurry, wherein, in water soluble resin and silicon carbide slurry, the weight ratio of silicon carbide is 12:100;
3) mixed with the first modified slurry by softening agent (triethyl citrate) and carry out ball milling 1.5h with obtained second modified slurry, wherein, in softening agent and silicon carbide slurry, the weight ratio of silicon carbide is 4:100;
4) mixed with the second modified slurry by releasing agent (white clay) and carry out ball milling 70min with obtained 3rd modified slurry, wherein, in releasing agent and silicon carbide slurry, the weight ratio of silicon carbide is 1.4:100;
5) the 3rd modified slurry is carried out spraying dry 80min (inlet temperature is 190 DEG C, and air outlet temperature is 140 DEG C) with obtained silicon carbide/molybdenumdisulphide composite ceramics A3.
Comparative example 1
Obtained composite ceramics B1 is carried out according to the method for embodiment 1, unlike, do not use graphite.
Comparative example 2
Obtained composite ceramics B2 is carried out according to the method for embodiment 1, unlike, do not use molybdenumdisulphide.
Comparative example 3
Obtained composite ceramics B3 is carried out according to the method for embodiment 1, unlike, do not use molybdenumdisulphide.
Comparative example 4
Obtained composite ceramics B4 is carried out according to the method for embodiment 1, unlike, do not use softening agent.
Comparative example 5
Obtained composite ceramics B5 is carried out according to the method for embodiment 1, unlike, do not use releasing agent.
Comparative example 6
Obtained composite ceramics B6 is carried out according to the method for embodiment 1, unlike, the particle diameter of silicon carbide is 0.5 μm.
Comparative example 7
Obtained composite ceramics B7 is carried out according to the method for embodiment 1, unlike, the particle diameter of silicon carbide is 10 μm.
Test example 1
Detect the rate of expansion of the bending strength of above-mentioned composite ceramics, fracture toughness property, shock strength and 200 DEG C, concrete outcome is in table 1.
Table 1
| Bending strength/Mpa | Fracture toughness property/Mpam 1/2 | Shock strength/Jcm -2 | Rate of expansion/the % of 200 DEG C | |
| A1 | 900 | 11 | 5.0 | 0.8 |
| A2 | 890 | 10 | 4.9 | 0.7 |
| A3 | 905 | 12 | 5.1 | 0.9 |
| B1 | 805 | 7 | 4.4 | 1.3 |
| B2 | 776 | 8 | 4.2 | 1.4 |
| B3 | 759 | 6 | 4.1 | 1.2 |
| B4 | 811 | 7 | 4.3 | 1.4 |
| B5 | 773 | 6 | 4.0 | 1.5 |
| B6 | 850 | 9 | 4.6 | 1.1 |
| B7 | 846 | 8 | 4.5 | 1.2 |
Known by the data in upper table, composite ceramics provided by the invention has the stability under excellent mechanical property and high temperature.
Test example 2
Detect above-mentioned composite ceramics frictional coefficient at each temperature, concrete outcome is in table 2.
Table 2
| Frictional coefficient at 100 DEG C | Frictional coefficient at 200 DEG C | Frictional coefficient at 300 DEG C | |
| A1 | 0.39 | 0.41 | 0.43 |
| A2 | 0.40 | 0.42 | 0.43 |
| A3 | 0.41 | 0.41 | 0.42 |
| B1 | 0.40 | 0.41 | 0.41 |
| B2 | 0.38 | 0.39 | 0.40 |
| B3 | 0.37 | 0.38 | 0.39 |
| B4 | 0.39 | 0.40 | 0.41 |
| B5 | 0.38 | 0.40 | 0.41 |
| B6 | 0.36 | 0.38 | 0.39 |
| B7 | 0.37 | 0.38 | 0.39 |
Known by the data in upper table, composite ceramics provided by the invention has lower frictional coefficient at low temperatures, at high temperature has higher frictional coefficient, i.e. antifriction during low temperature, increases and rub during high temperature.
Test example 3
Detect the wear rate Δ at above-mentioned composite ceramics at each temperature 100 DEG C
1(10
-7cm
3/ Nm), wear rate Δ at 200 DEG C
2(10
-7cm
3/ Nm) and 300 DEG C at wear rate Δ
3(10
-7cm
3/ Nm), concrete outcome is in table 3.
Table 3
| Δ 1(10 -7cm 3/Nm) | Δ 2(10 -7cm 3/Nm) | Δ 3(10 -7cm 3/Nm) | |
| A1 | 0.09 | 0.26 | 0.55 |
| A2 | 0.10 | 0.27 | 0.56 |
| A3 | 0.09 | 0.25 | 0.54 |
| B1 | 0.13 | 0.29 | 0.60 |
| B2 | 0.12 | 0.28 | 0.59 |
| B3 | 0.12 | 0.31 | 0.62 |
| B4 | 0.11 | 0.28 | 0.59 |
| B5 | 0.13 | 0.30 | 0.62 |
| B6 | 0.10 | 0.27 | 0.58 |
| B7 | 0.10 | 0.28 | 0.57 |
Known by the data in upper table, composite ceramics provided by the invention all has lower wearing and tearing at various temperatures.
More than describe the preferred embodiment of the present invention in detail; but the present invention is not limited to the detail in above-mentioned embodiment, within the scope of technical conceive of the present invention; can carry out multiple simple variant to technical scheme of the present invention, these simple variant all belong to protection scope of the present invention.
It should be noted that in addition, each concrete technical characteristic described in above-mentioned embodiment, in reconcilable situation, can be combined by any suitable mode, in order to avoid unnecessary repetition, the present invention illustrates no longer separately to various possible array mode.
In addition, also can carry out arbitrary combination between various different embodiment of the present invention, as long as it is without prejudice to thought of the present invention, it should be considered as content disclosed in this invention equally.
Claims (10)
1. silicon carbide/molybdenumdisulphide composite ceramics, is characterized in that, containing silicon carbide, graphite, molybdenumdisulphide, water soluble resin, softening agent and releasing agent;
Wherein, described water soluble resin be selected from urea-formaldehyde resin, terpolycyantoamino-formaldehyde resin, polyacrylic acid and polymethyl acrylic acid one or more, the particle diameter of described silicon carbide is 1-5 μm.
2. composite ceramics according to claim 1, wherein, the weight-average molecular weight of described water soluble resin is 2000-20000;
Preferably, described releasing agent be selected from silicone oil, paraffin, polyethylene wax, talcum powder, mica, potter's clay and white clay one or more, described softening agent be selected from phthalic acid ester compounds, aliphatic dibasic acid ester compound, phosphate compounds, polyol ester compounds, benzene polyacid ester compound and citric acid ester type compound one or more.
3. composite ceramics according to claim 1 and 2, wherein, relative to the described silicon carbide of 100 weight parts, the content of described graphite is 5-16 weight part, the content of described molybdenumdisulphide is 11-26 weight part, the content of described water soluble resin is 5-12 weight part, and the content of described softening agent is 1-4 weight part, and the content of described releasing agent is 0.5-1.4 weight part.
4. a preparation method for silicon carbide/molybdenumdisulphide composite ceramics, is characterized in that, comprising:
1) described silicon carbide, graphite, molybdenumdisulphide and water mixed and carry out grinding with obtained silicon carbide slurry;
2) water soluble resin mixed with described silicon carbide slurry and carry out grinding with obtained first modified slurry;
3) softening agent mixed with described first modified slurry and carry out grinding with obtained second modified slurry;
4) releasing agent mixed with described second modified slurry and carry out grinding with obtained 3rd modified slurry;
5) described 3rd modified slurry is carried out drying with obtained described silicon carbide/molybdenumdisulphide composite ceramics;
Wherein, described water soluble resin be selected from urea-formaldehyde resin, terpolycyantoamino-formaldehyde resin, polyacrylic acid and polymethyl acrylic acid one or more, the particle diameter of described silicon carbide is 1-5 μm.
5. preparation method according to claim 4, wherein, the weight-average molecular weight of described water soluble resin is 2000-20000;
Preferably, described releasing agent be selected from silicone oil, paraffin, polyethylene wax, talcum powder, mica, potter's clay and white clay one or more, described softening agent be selected from phthalic acid ester compounds, aliphatic dibasic acid ester compound, phosphate compounds, polyol ester compounds, benzene polyacid ester compound and citric acid ester type compound one or more.
6. the composite ceramics according to claim 4 or 5, wherein, relative to the described silicon carbide of 100 weight parts, the consumption of described graphite is 5-16 weight part, the consumption of described molybdenumdisulphide is 11-26 weight part, and the consumption of described water soluble resin is 5-12 weight part, and the consumption of described softening agent is 1-4 weight part, the consumption of described releasing agent is 0.5-1.4 weight part, and the consumption of described water is 99-170 weight part.
7. composite ceramics according to claim 6, wherein, the solid content of described silicon carbide slurry is 30 % by weight-40 % by weight.
8. composite ceramics according to claim 6, wherein, described grinding is ball milling.
9. composite ceramics according to claim 8, wherein, in step 1) in, the time of described grinding is 40-70min; In step 2) in, the time of described grinding is 1-2h; In step 3) in, the time of described grinding is 1-1.5h; In step 4) in, the time of described grinding is 40-70min.
10. the composite ceramics according to any one in claim 4,5,7,8 and 9, wherein, in step 5) in, described drying is spraying dry;
Preferably, described spraying dry at least meets the following conditions: inlet temperature is 170-190 DEG C, and air outlet temperature is 120-140 DEG C, and time of drying is 40-80min.
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| CN109265175A (en) * | 2018-10-22 | 2019-01-25 | 三明学院 | A kind of high-strength ceramic product and preparation method thereof |
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