阅读说明：本技术 一种蓝宝石及石墨烯掺杂生成蓝宝石的方法 (A kind of sapphire and graphene doping generate sapphire method ) 是由 承刚 卢铁成 齐建起 黄旭 魏念 石彦立 于 2019-10-08 设计创作，主要内容包括：本发明公开了一种石墨烯掺杂生成蓝宝石的方法,包括以下步骤：步骤①：将氧化铝粉料和石墨烯粉料混合均匀成混合料A待用；步骤②：将石墨烯粉料和氟化钾粉料混合均匀成混合料B待用；步骤③：将混合料A干压成型后烧结成饼料；步骤④：将饼料放入晶体生长装置,每层饼料上放置一层混合料B；步骤⑤：真空状态下升温化料成溶体,然后保温、降功率、搅拌至杂质层消失；步骤⑥：引晶；步骤⑦：晶体生长；步骤⑧：退火、自然冷却、开炉取晶体。本发明生长的石墨烯掺杂蓝宝石材料,与普通蓝宝石材料相比具有更好的高温强度,更宽的介电常数调节范围,更小的介电损耗,是一种良好的新型微波窗口材料。(The invention discloses a kind of doping of graphene to generate sapphire method, comprising the following steps: step 1.: it is stand-by that alumina powder and graphene powder are mixed into mixture A；Step is 2.: it is stand-by that graphene powder and potassium fluoride powder being mixed into mixture B；Step is 3.: by mixture A it is dry-pressing formed after sinter biscuit into；Step is 4.: biscuit being put into crystal growing apparatus, places one layer of mixture B on every layer cake material；Step is 5.: under vacuum state then temperature increasing for melting materials keeps the temperature at solution, drops power, stirring to impurity layer disappears；Step is 6.: seeding；Step is 7.: crystal growth；Step is 8.: annealing, natural cooling, blow-on take crystal.The graphene that the present invention is grown adulterates sapphire material, has better elevated temperature strength compared with common sapphire material, broader dielectric constant adjustable range, smaller dielectric loss is a kind of good novel microwave window material.)

1. a kind of sapphire, it is characterised in that: the sapphire is generated by aluminium oxide and graphene.

2. a kind of graphene doping generates sapphire method, comprising the following steps:

Step is 1.: it is stand-by that alumina powder and graphene powder being mixed into mixture A；

Step is 2.: it is stand-by that graphene powder and potassium fluoride powder being mixed into mixture B；

Step is 3.: by mixture A it is dry-pressing formed after sinter biscuit into；

Step is 4.: biscuit being put into crystal growing apparatus, places one layer of mixture B on every layer cake material；

Step is 5.: under vacuum state then temperature increasing for melting materials keeps the temperature at solution, drops power, stirring to impurity layer disappears；

Step is 6.: seeding；

Step is 7.: crystal growth；

Step is 8.: annealing, natural cooling, blow-on take crystal.

3. graphene according to claim 2 doping generates sapphire method, it is characterised in that: the step 1. in, Graphene powder measures≤0.1% alumina powder weight again.

4. graphene doping according to claim 3 generates sapphire method, it is characterised in that: the graphene is single The graphene of layer, Du≤1 micron graphene Li.

5. generating sapphire method according to any graphene doping of claim 2-4, it is characterised in that: the step 2. in, graphene powder and potassium fluoride weight ratio are 1:1.

6. generating sapphire method according to any graphene doping of claim 2-5, it is characterised in that: the step 3. in, sintering temperature is 1800 DEG C -1850 DEG C.

7. generating sapphire method according to any graphene doping of claim 2-6, it is characterised in that: the step 4. in, the mixture B: mixture A weight ratio is 0.1%-0.5%.

8. generating sapphire method according to any graphene doping of claim 2-6, it is characterised in that: the step In 5., vacuum state be 0.1 atmospheric pressure hereinafter, temperature increasing for melting materials at solution be 6-10 one-hour rating rise to 50 kilowatts of progress materials at Melt, soaking time are 3-5 hours, and the time for stirring beginning is that power is down to 45-47 kilowatt hour.

9. generating sapphire method according to any graphene doping of claim 2-8, it is characterised in that: the step 6. in, seeding is slowly to be put into seed crystal in melt, and seed crystal is developed to 50-60mm at pull rate 1mm/5min.

10. generating sapphire method according to any graphene doping of claim 2-9, it is characterised in that: the crystalline substance Power drops 40 watts until crystal development is to diameter 100mm per hour when body is grown to growth, and then power drops 50 watts directly per hour To crystal development to diameter 200m.

Technical field

The invention belongs to sapphire preparation fields, and in particular to a kind of sapphire and graphene doping generate sapphire side Method.

Background technique

Sapphire group becomes aluminium oxide (Al2O3), is by three oxygen atoms and two aluminium atoms with covalent bond pattern knot It closes, crystal structure is hexagonal lattice structure.Since sapphire has the high velocity of sound, high temperature resistant, anticorrosive, high rigidity, height The features such as translucency, fusing point high (2045 DEG C), therefore often it is used as the material of photoelectric cell.Super brightness is white/blue at present The quality of light LED depend on epitaxial layer of gallium nitride (GaN) material quality, and epitaxial layer of gallium nitride quality then with used indigo plant Jewel substrate surface processing quality is closely bound up.Due to the face sapphire (monocrystalline Al2O3) c and III-V and II-VI race's deposition film Between lattice constant mismatch rate it is small, while meeting requirement resistant to high temperature in GaN epitaxy processing procedure, so that sapphire wafer becomes system Make the critical material of white/blue green light LED.

The growing method of sapphire crystal material at present there are many kinds of, mainly have: kyropoulos (i.e. Kyropolos method, letter Claim KY method), EFG technique (i.e. edge defined film-fed growth techniques method, abbreviation EFG method), heat exchange Method (i.e. heat exchange method method, abbreviation HEM method), czochralski method (i.e. Czochralski, abbreviation Cz method), cloth Ritchie Graceful method (i.e. Bridgman method or Bridgman-Stockbarger method) etc..

Summary of the invention

One of the objects of the present invention is to provide a kind of sapphires.

Technical solution is: a kind of sapphire, which is generated by aluminium oxide and graphene.

The second object of the present invention is to provide a kind of graphene doping and generates sapphire method, this method material time Short, stress is small.

A kind of doping of graphene generates sapphire method, comprising the following steps: step 1.: by alumina powder and graphite It is stand-by that alkene powder is mixed into mixture A；Step is 2.: graphene powder and potassium fluoride powder are mixed into mixture B For use；Step is 3.: by mixture A it is dry-pressing formed after sinter biscuit into；Step is 4.: biscuit is put into crystal growing apparatus, every layer One layer of mixture B is placed on biscuit；Step is 5.: under vacuum state then temperature increasing for melting materials keeps the temperature at solution, drops power, stirring extremely Impurity layer disappears；Step is 6.: seeding；Step is 7.: crystal growth；Step is 8.: annealing, natural cooling, blow-on take crystal.

Preferably, the step 1. in, graphene powder measures≤0.1% alumina powder weight again.

Preferably, the graphene is the graphene of single layer, Du≤1 micron graphene Li.

Preferably, the step 2. in, graphene powder and potassium fluoride weight ratio are 1:1.

Preferably, the step 3. in, sintering temperature be 1800 DEG C -1850 DEG C.

Preferably, the step 4. in, the mixture B: mixture A weight ratio be 0.1%-0.5%.

Preferably, the step 5. in, vacuum state is 0.1 atmospheric pressure hereinafter, temperature increasing for melting materials at solution is 6-10 small When power rise to 50 kilowatts of progress materials into melt, soaking time is 3-5 hour, stirs the time of beginning and for power is down to 45- 47 kilowatt hours.

Preferably, the step 6. in, seeding be seed crystal is slowly put into melt, at pull rate 1mm/5min Seed crystal is developed to 50-60mm.

Preferably, when the crystal growth is growth power drop per hour 40 watts until crystal development to diameter 100mm, Then power drops 50 watts up to crystal development to diameter 200m per hour.

Compared with prior art, inventive principle of the present invention and the utility model has the advantages that

Inventor it has been investigated that, two steps addition graphene can prevent graphene from volatilizing, addition potassium fluoride can To increase the solubility in material stage and the stability of seeding and follow-up phase lattice, low growth rate and long annealing time can To reduce stress, graphene is adjustable sapphire dielectric properties, improves thermodynamic property and processing performance, what the present invention generated Sapphire can be used as particular/special requirement such as high temperature, the window material of microwave.

Specific embodiment

The invention will be further described below.

A kind of sapphire method of graphene doping generation, comprising the following steps:

Step is 1.: it is stand-by that alumina powder and graphene powder being mixed into mixture A；Graphene powder measures again≤ 0.1% alumina powder weight.

Step is 2.: it is stand-by that graphene powder and potassium fluoride powder being mixed into mixture B；The graphene is single layer Graphene, Du≤1 micron graphene Li.Graphene powder and potassium fluoride weight ratio are 1:1.Graphene number of plies is excessive or stone Black alkene granularity is greater than 1 micron, may generate bubble.

Step is 3.: by mixture A it is dry-pressing formed after sinter biscuit into；Sintering temperature is 1800 DEG C -1850 DEG C.

Step is 4.: biscuit being put into crystal growing apparatus, places one layer of mixture B on every layer cake material；The mixture B: Mixture A weight ratio is 0.1%-0.5%.

Step is 5.: under vacuum state then temperature increasing for melting materials keeps the temperature at solution, drops power, stirring to impurity layer disappears；Vacuum State is 0.1 atmospheric pressure hereinafter, temperature increasing for melting materials at solution is that 6-10 one-hour rating rises to 50 kilowatts of progress materials into melt, heat preservation Time is 3-5 hours, and the time for stirring beginning is that power is down to 45-47 kilowatt hour.

Step is 6.: seeding；Seeding is slowly to be put into seed crystal in melt, develops seed crystal at pull rate 1mm/5min To 50-60mm.

Step is 7.: crystal growth；Power drops 40 watts up to crystal development to diameter per hour when crystal growth is growth 100mm, then power drops 50 watts up to crystal development to diameter 200m per hour.

Step is 8.: annealing, natural cooling, blow-on take crystal.