CN106518088A - Manufacturing method of high-performance silicon nitride sealing ring - Google Patents
Manufacturing method of high-performance silicon nitride sealing ring Download PDFInfo
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- CN106518088A CN106518088A CN201610955908.7A CN201610955908A CN106518088A CN 106518088 A CN106518088 A CN 106518088A CN 201610955908 A CN201610955908 A CN 201610955908A CN 106518088 A CN106518088 A CN 106518088A
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
- C04B35/584—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on silicon nitride
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B28—WORKING CEMENT, CLAY, OR STONE
- B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
- B28B3/00—Producing shaped articles from the material by using presses; Presses specially adapted therefor
- B28B3/003—Pressing by means acting upon the material via flexible mould wall parts, e.g. by means of inflatable cores, isostatic presses
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Abstract
The invention discloses a manufacturing method of a high-performance silicon nitride sealing ring. The manufacturing method comprises the following steps: 1, preparing raw materials: silicon nitride powder, magnesium oxide, aluminum oxide and yttrium oxide; 2, adding the raw materials and an adhesive to absolute ethyl alcohol and mixing uniform so as to obtain silicon nitride composite powder slurry; 3, carrying out spray granulation on the silicon nitride composite powder slurry by adopting a closed-ring granulation mode so as to prepare silicon nitride granulated powder; 4, carrying out cool isostatic pressing treatment molding after carrying out compression molding on the silicon nitride granulated powder so as to prepare a silicon nitride ring blank; and 5, sintering the silicon nitride ring blank at a 1-8MPa nitrogen atmosphere and 1750-1850DEG C to prepare the silicon nitride sealing ring. The relative density of the made silicon nitride sealing ring is larger than or equal to 99.5%, the strength is larger than or equal to 800MPa, the HV hardness is larger than or equal to 1600, and the fracture toughness can reach 6.5-7.5MPa.m<1/2>. The manufacturing method greatly meets the application of the silicon nitride material in the aspects of sealing ring markets, particularly mechanical sealing.
Description
Technical field
The present invention relates to a kind of preparation method of high-performance silicon nitride sealing ring.
Background technology
In mechanical seal, static and dynamic sealing ring generally requires to resist wash away shock, high rotating speed, the high pressure of solid particle and brings
Sealing surface seal parameters are unstable, the unfavorable factor such as basal body structure part is corroded impact.For meet mechanical seal low abrasion,
Long life requirement, generally requires seal ring material and has high rigidity, high-fracture toughness and high rigidity（Elastic modelling quantity）.
Silicon nitride ceramics is a kind of new seal ring material, has compared to hard alloy seal ring that density is low, corrosion resistant
The advantages of erosion, there is high intensity, high fracture toughness and excellent resistance to than aluminium oxide ceramics sealing ring, silicon carbide sealed ring
Polishing machine, especially under the conditions of water or alcoholic medium, silicon nitride sealing ring can form SiO films due to friction surface, with good
Good self lubricity, coefficient of friction is little, wear rate is low, with excellent wearability and long service life.
As silicon nitride material self-diffusion coefficient is low, itself sinters difficulty, generally requires high temperature（More than 1900 DEG C）Or
High pressure could densified sintering product, but silicon nitride material at high temperature and extremely easily decomposes.At present, high-performance silicon nitride sealing ring master
Hot pressing to be passed through, HIP sintering are prepared from.Hot pressing, HIP sintering are by applying to product in product sintering process
Plus-pressure promotes the densification of material（What hot pressing applied is axial mechanical force, and high temperature insostatic pressing (HIP) is the gas by 200MPa pressure
Uniform pressurization）.But hot pressing, HIP sintering not only need agglomerating plant costly, and sinter cost（Water, electricity,
Gas, auxiliary consumptive material such as jacket etc.）Height, has been significantly greatly increased the manufacturing cost of silicon nitride product, has contained high-performance silicon nitride material
Application on sealing ring market.
The content of the invention
It is an object of the invention to provide a kind of preparation method of high-performance silicon nitride sealing ring, silicon nitride system obtained in which
Its fracture toughness of product is far above hot pressing, high temperature insostatic pressing (HIP) product, and its preparation cost is far below hot pressing, HIP sintering.
For achieving the above object, the technical solution used in the present invention is as follows：
A kind of preparation method of high-performance silicon nitride sealing ring, comprises the following steps：
（1）Prepare raw material by following weight ratio：Silicon nitride powder 90～95%, magnesium oxide 0～1%, aluminium oxide 2～4%, yittrium oxide 3～
7%；
（2）Raw material, binding agent are added in dehydrated alcohol, are then mixed, be configured to the silicon nitride that solid concentration is 40～50%
Composite powder slip；The weight of described adhesive for raw material weight 0.5～2.5%；
（3）Mist projection granulating is carried out to silicon nitride composite powder slurry using closed loop pelletize mode, silicon nitride pelletizing is obtained；
（4）Pour silicon nitride pelletizing into sealing ring mould, 120 are then carried out after compression molding under the pressure of 20～80MPa
～250MPa isostatic cool pressings process molding, and silicon oxide ring billet body is obtained；
（5）Silicon nitride ring billet body is sintered under the conditions of 1～8MPa nitrogen atmospheres, 1750～1850 DEG C, silicon nitride is obtained
Sealing ring.
Further, the step（2）In, raw material, adhesive and dehydrated alcohol are mixed by the way of ball milling.
Preferably, the ball, material ratio 2～3: the 1 during ball milling.
Preferably, the adhesive be Polyethylene Glycol, in polyvinyl alcohol carboxylic butyraldehyde it is arbitrary one or two.
Yet further, the step（3）In, the process conditions of mist projection granulating are nitrogen atmosphere, inlet temperature 150～
190 DEG C, 65～90 DEG C of outlet temperature.
Compared with prior art, the invention has the advantages that：
（1）The present invention is by applying the nitrogen of 1～8MPa, it is suppressed that the decomposition under silicon nitride high temperature so that silicon nitride can be
Higher temperature（≥1750℃）Under be sintered；Simultaneously added with effect sintering aid（Aluminium oxide and yittrium oxide）, promote silicon nitride
While densification, also promote the growth of silicon nitride middle long column shape beta silicon nitride crystal grain, so as to the power of silicon nitride material is greatly improved
Learn performance.Practice have shown that, the silicon nitride sealing ring relative density that the present invention is prepared is more than or equal to 99.5%, intensity is more than
Or 800MPa is equal to, HV hardness is more than or equal to 1600, and fracture toughness can reach 6.5～7.5 MPa m1/2, therefore, by this
Silicon nitride product obtained in invention, its not only fracture toughness be far above hot pressing, high temperature insostatic pressing (HIP) product, and preparation cost is far below
Hot pressing, HIP sintering.
（2）As mechanical seal ring has strict demand to the uniformity of seal ring material component of organization, therefore, it is to ensure system
The good composition structural homogenity of product, present invention employs closed loop granulation powder handling process and cold isostatic compaction technique, has
Help the uniformity of silicon nitride sealing ring component of organization.
Specific embodiment
With reference to embodiment, the invention will be further described, and the mode of the present invention includes but are not limited to following enforcement
Example.
The invention provides a kind of new silicon nitride sealing ring preparation technology, which is with silicon nitride powder as raw material, and is aided with
Magnesium oxide, aluminium oxide and yittrium oxide realize the high densification sintering of silicon nitride material as sintering aid.The concrete technology of the present invention
Flow process is as follows：
（1）By weight preparation raw material：Silicon nitride powder 90～95%, magnesium oxide 0～1%, aluminium oxide 2～4%, yittrium oxide 3～7%；
（2）By raw material, binding agent（In Polyethylene Glycol, polyvinyl alcohol carboxylic butyraldehyde it is arbitrary one or two）It is added to dehydrated alcohol
In, then mix, be configured to the silicon nitride composite powder slip that solid concentration is 40～50%；The weight of described binding agent is original
The 0.5～2.5% of material weight；Raw material, binding agent and dehydrated alcohol are mixed by the way of ball milling by the present embodiment, and ball, material ratio
2～3: 1；
（3）Mist projection granulating is carried out to silicon nitride composite powder slurry using closed loop pelletize mode, silicon nitride pelletizing is obtained；Spraying is made
Grain process conditions be nitrogen atmosphere, 150～190 DEG C of inlet temperature, 65～90 DEG C of outlet temperature；
（4）Pour silicon nitride pelletizing into sealing ring mould, 120 are then carried out after compression molding under the pressure of 20～80MPa
～250MPa isostatic cool pressings process molding, and silicon oxide ring billet body is obtained；
（5）Silicon nitride ring billet body is sintered under the conditions of 1～8MPa nitrogen atmospheres, 1750～1850 DEG C, silicon nitride is obtained
Sealing ring.
The silicon nitride sealing ring relative density that the present invention is prepared is more than or is equal to 99.5%, and intensity is more than or equal to
800MPa, HV hardness is more than or equal to 1600, and fracture toughness can reach 6.5～7.5 MPa m1/2.Below with several examples pair
The effect of the present invention is illustrated.
Example 1
Silicon nitride powder, magnesium oxide, aluminium oxide, the weight ratio respectively 93%, 4%, 0.5% and 2.5% of yittrium oxide, will be four compositions mixed
Powder is closed, the 1% of mixed powder weight PVB mixing is subsequently adding, is obtained mixture.Then, according to mixture: abrading-ball: dehydrated alcohol
=1: 2.5: 1.2 weight is poured in agitating ball mill, ball milling 6 hours than configuration abrading-ball and dehydrated alcohol, obtains silicon nitride multiple
Close slurry material.
Then, pelletize will be carried out in silicon nitride composite powder slurry suction to closed loop granulation tower, technique is N2Atmosphere, import temperature
170 DEG C of degree, 70 DEG C of outlet temperature obtains silicon nitride pelletizing；
Pour the silicon nitride pelletizing for obtaining into sealing ring mould, 150MPa isostatic cool pressings are carried out after 20MPa molding preforming
Molding is processed, high density silicon nitride sealing ring base substrate is obtained.
Finally, by above-mentioned silicon nitride sealing ring base substrate in 1700 DEG C, 1MPa and 1800 DEG C, the N of 6MPa2It is complete under atmospheric condition
Into sintering, silicon nitride sealing ring is obtained.
Silicon nitride sealing ring obtained in this example, its relative density are 99.7%, and intensity is more than or equal to 800 MPa, hardness
（HV）More than or equal to 1650, fracture toughness is 7.0 MPa m1/2。
Example 2
Silicon nitride powder, magnesium oxide, aluminium oxide, the weight ratio respectively 90%, 5.5%, 1% and 3.5% of yittrium oxide, will be four compositions mixed
Powder is closed, the PEG mixing of the 1% of mixed powder weight PVB and 1% is subsequently adding, is obtained mixture.Then, according to mixture: abrading-ball
: dehydrated alcohol=1: 3: 1.5 weight is poured in agitating ball mill, ball milling 4 hours, obtains nitrogen than configuration abrading-ball and dehydrated alcohol
SiClx composite powder slurry.
Then, pelletize will be carried out in silicon nitride composite powder slurry suction to closed loop granulation tower, technique is N2Atmosphere, import temperature
185 DEG C of degree, 80 DEG C of outlet temperature obtains silicon nitride pelletizing；
Pour the silicon nitride pelletizing for obtaining into sealing ring mould, 170MPa isostatic cool pressings are carried out after 40MPa molding preforming
Molding is processed, high density silicon nitride sealing ring base substrate is obtained.
Finally, by above-mentioned silicon nitride sealing ring base substrate in 1700 DEG C, 0.5MPa and 1780 DEG C, the N of 3MPa2Under atmospheric condition
Sintering is completed, silicon nitride sealing ring is obtained.
Silicon nitride sealing ring obtained in this example, its relative density are 99.8%, and intensity is more than or equal to 830 MPa, hardness
（HV）More than or equal to 1610, fracture toughness is 6.7 MPa m1/2。
Example 3
Silicon nitride powder, magnesium oxide, aluminium oxide, the weight ratio respectively 95%, 2.5%, 1% and 1.5% of yittrium oxide, will be four compositions mixed
Powder is closed, the PEG mixing of the 0.5% of mixed powder weight PVB and 2% is subsequently adding, is obtained mixture.Then, according to mixture: mill
Ball: dehydrated alcohol=1: 2: 1 weight is poured in agitating ball mill, ball milling 8 hours, obtains nitrogen than configuration abrading-ball and dehydrated alcohol
SiClx composite powder slurry.
Then, pelletize will be carried out in silicon nitride composite powder slurry suction to closed loop granulation tower, technique is N2Atmosphere, import temperature
155 DEG C of degree, 60 DEG C of outlet temperature obtains silicon nitride pelletizing；
Pour the silicon nitride pelletizing for obtaining into sealing ring mould, 200MPa isostatic cool pressings are carried out after 60MPa molding preforming
Molding is processed, high density silicon nitride sealing ring base substrate is obtained.
Finally, by above-mentioned silicon nitride sealing ring base substrate in 1700 DEG C, 1.5MPa and 1850 DEG C, the N of 8MPa2Under atmospheric condition
Sintering is completed, silicon nitride sealing ring is obtained.
Silicon nitride sealing ring obtained in this example, its relative density are 99.6%, and intensity is more than or equal to 900 MPa, hardness
（HV）More than or equal to 1680, fracture toughness is 7.3 MPa m1/2。
It is for the present invention compares existing process, not only with low cost, and technological process is simple, efficiency high.The present invention is logical
The reasonable selection and proportioning of raw material are crossed, with reference to the sintering process of design, the mechanical property of silicon nitride material is greatly improved, fully
Meet application of the silicon nitride material in terms of sealing ring market, particularly mechanical seal.Therefore, the technology of the present invention progress is bright
It is aobvious, with prominent substantive distinguishing features and significant progress.
Above-described embodiment is only one of the preferred embodiment of the present invention, should not be taken to limit the protection model of the present invention
Enclose, all body design thought and changes or polishing for having no essential meaning for mentally making in the present invention, what which was solved
Technical problem is still consistent with the present invention, should be included within protection scope of the present invention.
Claims (5)
1. a kind of preparation method of high-performance silicon nitride sealing ring, it is characterised in that comprise the following steps：
（1）Prepare raw material by following weight ratio：Silicon nitride powder 90～95%, magnesium oxide 0～1%, aluminium oxide 2～4%, yittrium oxide 3～
7%；
（2）Raw material, binding agent are added in dehydrated alcohol, are then mixed, be configured to the silicon nitride that solid concentration is 40～50%
Composite powder slip；The weight of described adhesive for raw material weight 0.5～2.5%；
（3）Mist projection granulating is carried out to silicon nitride composite powder slurry using closed loop pelletize mode, silicon nitride pelletizing is obtained；
（4）Pour silicon nitride pelletizing into sealing ring mould, 120 are then carried out after compression molding under the pressure of 20～80MPa
～250MPa isostatic cool pressings process molding, and silicon oxide ring billet body is obtained；
（5）Silicon nitride ring billet body is sintered under the conditions of 1～8MPa nitrogen atmospheres, 1750～1850 DEG C, silicon nitride is obtained
Sealing ring.
2. a kind of preparation method of high-performance silicon nitride sealing ring according to claim 1, it is characterised in that the step
（2）In, raw material, adhesive and dehydrated alcohol are mixed by the way of ball milling.
3. a kind of preparation method of high-performance silicon nitride sealing ring according to claim 2, it is characterised in that the ball milling
When ball, material ratio 2～3: 1.
4. the preparation method of a kind of high-performance silicon nitride sealing ring according to Claims 2 or 3, it is characterised in that described
Adhesive is Polyethylene Glycol, in polyvinyl alcohol carboxylic butyraldehyde it is arbitrary one or two.
5. a kind of preparation method of high-performance silicon nitride sealing ring according to claim 1, it is characterised in that the step
（3）In, the process conditions of mist projection granulating are nitrogen atmosphere, 150～190 DEG C of inlet temperature, 65～90 DEG C of outlet temperature.
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| CN201610955908.7A CN106518088A (en) | 2016-10-27 | 2016-10-27 | Manufacturing method of high-performance silicon nitride sealing ring |
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| CN114085084A (en) * | 2020-08-25 | 2022-02-25 | 西安增材制造国家研究院有限公司 | High-strength silicon nitride ceramic and preparation method thereof |
| CN114986661A (en) * | 2022-04-07 | 2022-09-02 | 辽宁伊菲科技股份有限公司 | Preparation method and device of silicon nitride sonar thermal imaging insulating strip |
| CN117303913A (en) * | 2023-10-19 | 2023-12-29 | 衡阳凯新特种材料科技有限公司 | High-performance silicon nitride sealing ring and preparation method thereof |
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| CN113929472A (en) * | 2021-11-24 | 2022-01-14 | 福州赛瑞特新材料技术开发有限公司 | Preparation method of composite boron nitride ceramic nozzle |
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